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CAS No. : | 35963-20-3 | MDL No. : | MFCD00064158 |
Formula : | C10H16O4S | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | MIOPJNTWMNEORI-XVKPBYJWSA-N |
M.W : | 232.30 | Pubchem ID : | 5771688 |
Synonyms : |
|
Signal Word: | Danger | Class: | 8 |
Precautionary Statements: | P501-P260-P264-P280-P303+P361+P353-P301+P330+P331-P363-P304+P340+P310-P305+P351+P338+P310-P405 | UN#: | 3261 |
Hazard Statements: | H314 | Packing Group: | Ⅱ |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
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With hydrogenchloride; d-phenylglycine | ||
With brucine |
Yield | Reaction Conditions | Operation in experiment |
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With thionyl chloride; for 12h;Reflux; | General procedure: (1S)-(+)-Camphor-10-sulfonic acid (1.16 g, 5 mmol) was refluxed in thionyl chloride (8 mL) for 12 h. Then, the excess thionyl chloride was removed under reduced pressure to afford (1S)-(+)-10-camphorsulfonyl chloride, which was used in the next step without purification. |
Yield | Reaction Conditions | Operation in experiment |
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6 The absolute stereochemistry of cycloprop[d]indolo[2,1-a][2]benzazepine-5-carboxamide, 8-cyclohexyl-N-[(dimethylamino)sulfonyl]-1,1a,2,12b-tetrahydro-11-methoxy-1a-[(3-methyl-3,8-diazabicyclo[3.2.1]oct-8-yl)carbonyl]-, (1aR,12bS)-rel-(-)- is as drawn above, and was determined from an x-ray crystal structure obtained on the (R)-camphorsulfonic acid salt. |
Yield | Reaction Conditions | Operation in experiment |
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84% | In tert-butyl methyl ether; isopropyl alcohol at 25℃; for 2h; | 1 13g (0.0316mol) of S-(-)-amlodipine was dissolved in 120 ml of isopropanol. 6.96g(1.05 eq.) of (lR)-(-)-10-camphorsulfonic acid was added to this solution and dissolved therein. Subsequently, to this solution was added 200 ml of t-butyl methyl ether, followed by stirring at 25 C for 2 hours to afford a precipitate. After filtration, the precipitate was washed and purified with 50 ml of t-butyl methyl ether and dried in a vacuum to produce 16.7 g of an anhydrate of S-(-)-amlodipine (lR)-(-)-10-camsylate as a white crystalline solid (yield: 84%, water content: 0.15%).[57] The anhydrate of crystalline S-(-)-amlodipine (lR)-(-)-10-camsylate was analyzed to determine diffraction angles using an X-ray powder diffraction method, and measured for melting point with an increase in temperature at a rate of l°C/min from50 to 2000C through a melting point measurement method (Melting Point Method I ofGeneral Test Methods in Korean Pharmacopeia D or Melting Point-Capillary Method ofEuropean Pharmacopoeia IV). [58] The X-ray diffraction spectrum of anhydrate of the above produced crystalline S-(-)-amlodipine (lR)-(-)-10-camsylate is shown in FIG. 1, and its elemental analysis data and melting point are given as follows. [59] - Diffraction Angles: 7.80°, 9.18°, 9.56°, 11.38°, 12.78°, 13.10°, 13.84°, 15.48°,15.68°, 17.38°, 18.94°, 19.92°, 21.78°, 23.16°, 24.64°, 25.86°, 26.44°, [60] - Elemental Analysis for C H ClN O S [found(%) (C: 56.11, H: 6.59, N: 4.36,J 30 42 2 9O: 22.42), calculated(%) (C: 56.30, H: 6.62, N: 4.30, O: 22.50)],[61] - m.p.(Melting point): 94-990C. |
83% | In water at 25℃; for 2h; | 2 13g (0.0316mol) of S-(-)-amlodipine was slurried with 200 ml of distilled water, followed by the addition of 6.96 g (1.05 eq.) of (lR)-(-)-10-camphorsulfonic acid thereto. Stirring for 2 hours at normal temperature formed a crystalline precipitate in the complete solution at a temperature of 250C. After filtration, the crystalline precipitate was washed with 20 ml of distilled water and dried at 4O0C in a vacuum to afford 16.62 g of S-(-)-amlodipine (lR)-(-)-10-camsylate anhydride (yield: 83%, water content: 0.34%).[66] The elemental analysis data and melting point of the anhydrate of crystalline S-(-)-amlodipine (lR)-(-)-10-camsylate are given as follows.[67] - Elemental analysis for C H ClN O S [found(%) (C: 56.11, H: 6.59, N: 4.36,O: 22.42), calculated(%) (C: 56.22, H: 6.65, N: 4.32, O: 22.55)].[68] - m.p.: 94-990C.[69] |
62.3% | In water; isopropyl alcohol at 15 - 20℃; | 1 Reference Example 1 : Preparation of S-(-)-amlodipine (RVcamsylate; 1O g of (S)-amlodipine free base obtained in Preparation 2 and 5.68 g of (R)-camρhor sulfonic acid were dissolved in 20 mi of isopropanol, to which 200 m£ of distilled water was slowly added dropwise. The resulting solution was stirred at room temperature overnight, cooled to 15 °C, and further stirred for 1 hour. The precipitated solid was filtered, washed with 25 mi of an isopropanol-water mixture (1 :10, v/v), and dried under a warm air flow at 40 °C, to obtain 9.77 g (yield: 62.3%) of the title compound in the form of a white solid.Optical purity: > 99.9% ee Moisture content: 3.2% |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 4 steps 1: SOCl2 2: NH3 / dioxane; H2O 3: 100 percent / NaBH4 / methanol; H2O 4: 90 percent / NaH / toluene; various solvent(s) / 20 °C | ||
Multi-step reaction with 5 steps 1: 80.5 percent / PCl5 / 1 h at 0 deg C and 2 h at r.t. 2: 74 percent / NH3 / toluene / 0 °C 3: 99.3 percent / NaOMe / methanol / 64 h / Ambient temperature 4: 1.) LiAlH4; 2.) 1N aq. HCl / 1.) THF, 0 deg C, 2.) r.t., 1 h 5: 88 percent / NaH / toluene / 3 h / Ambient temperature |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
25.7 - 31.0% | In ethanol; ethyl acetate; at 5 - 70℃; | Preparation of S- (-)-3- (1-DIMETHYLAMINO) PHENOL (III) Resolving compound (IV) with an 1 equivalent amount OF S- (+)-CAMPHOR-10-SULFONIC acid A solution of compound (IV) in ethylacetate (0.505 mol) * in 500 ml of ethylacetate) is introduced into a 1-liter round flask with a magnetic stirrer and a solution OF S- (+)-CAMPHOR- 10-sulfonic acid (117.4 g (0.505 mol) IN 250 ml of anhydrous ethanol), prepared in warm conditions, is added. The solution is inoculated and left to stand in a refrigerator (+5 C) overnight. The precipitated crystals are sucked off through fritted glass and left to air dry overnight. 1) 82.2 g of white crystals with m. p. = 165-171 C are obtained, which are dissolved in 190 ml of absolute ethanol under reflux. 380 ml of ethylacetate are added under warm conditions and crystallization is performed according to the above-mentioned procedure. 2) 64.1 g of white crystals with m. p. = 174-176 C are obtained, which are dissolved in 150 ML OF ETHANOL (ABSOL. ) UNDER REFLUX AND 300 ML OF ETHYLACETATE ARE ADDED UNDER WARM conditions. 3) 56.5 g of white crystals with m. p. = 177-179 C are obtained, which are dissolved in 130 ML OF ETHANOL (ABSOL. ) UNDER REFLUX AND 260 ML OF ETHYLACETATE ARE ADDED UNDER WARM conditions. 4) 51.6 g of white crystals with m. p. = 179-181 C are obtained; i. e. 25.7 % of the theoretical amount. * the contents of compound (IV) was determined by titration Resolving compound (IV) with 0.6 equivalent amount OF S- (+)-CAMPHOR-10-SULFONIC acid 100 g (0.605 mol) of compound (IV) are dissolved in 600 ml of ethylacetate under stirring and reflux. A solution of S- (+)-CAMPHOR-10-SULFONIC acid (84.3 g (0.363 mol) in 125 ML of anhydrous ethanol) is added under stirring at 70 C. The solution is inoculated, left to cool down to room temperature under stirring, cooled down with brine to-10 up TO-15C and it is left to crystallize for at least 12 hours under exclusion of air humidity. The precipitated first fraction of crystals is sucked off and air dried. 1) 95.0 g of white crystals with m. p. =173-175 C are obtained, which are dissolved in 175 ml of ethanol under stirring and reflux and 350 ml of ethylacetate are added at a temperature of the solution between 60-70 C. The CAMPHORSULFONATE will start to crystallize and is left to crystallize at a temperature-5 up to-10 C for at least 12 hours. The precipitated fraction is sucked off, washed with 2x 50 ml of ethylacetate and air dried. 2) 79.5 g of the second fraction with m. p. 176-178 C are obtained, which are again recrystallized in a mixture of ethanol: ethylacetate (150 ML : 300 ml) following the above specified procedure. After being washed with 2x 50 ml of ethylacetate, the product is dried freely. 3) 74.6 g of the third fraction with m. p. =177-179 C are obtained; i. e. 31.0 % of the theoretical yield. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
35% | In water; acetone; at 20℃; for 20 - 24h;Resolution of racemate; | 36.7 g of a racemic mixture containing the R(-)-I and S(+)-I enantiomers are resuspended with stirring in 200 ml of an acetone/water mixture (80/20). Then, 23 g (1.1 equivalents) of L-10-camphorsulfonic acid are added, and it is stirred until dissolution. The solution is seeded with the (-)L-10-camphorsulfonic-R(-)-I salt [I(-)C(-)], by means of which the solution begins to become cloudy, it is maintained with stirring at room temperature for 20-24 hours and is filtered. The solid obtained is resuspended again in 5 volumes of acetone/water (80/20), first under reflux and then at room temperature, for 20-24 hours, and is filtered again. The product obtained is dried to give 20.1 g of the I(-)C(-) salt, with a 35% yield. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
46.89 g of a racemic mixture of R(-)-I and S(+)-I resuspended in 705 ml of acetone with 5% water are heated to 40-45 C., and 18.6 g (0.7 equivalents) of D-10-camphorsulfonic acid are incorporated. Once it is all dissolved under heat, it is left to cool at room temperature, seeding with the (+) salt of D-10-camphorsulfonic-S(+)-I [I(+)C(+)] acid. The suspension obtained is left to stir at room temperature for 20-24 hours and is filtered. The residue obtained from the mother liquors is resuspended in 705 ml of dichloromethane and 705 ml of 7% NaHCO3, and is stirred until dissolution. [0083] After separating the phases, the organic phase is taken to residue and is replaced by 235 ml of acetone containing 20% water, to which 29.33 g (1.1 equivalents) of L-10-camphorsulfonic acid are added, stirring until dissolution. [0084] It is seeded with the L-10-camphorsulfonic-R(-)-I (-) salt [I(-)C(-)], by means of which the solution begins to become cloudy, it is maintained with stirring at room temperature for 20-24 hours and is filtered. The solid obtained is resuspended in 5 volumes of acetone containing 20% water, it is taken to reflux for 30 minutes, it is left stirring at 20-25 C. for 20 hours, is filtered and dried to give 17.65 g (0.027 moles, 24% yield) of a white solid. [0085] The optical purity of the R(-)-I enantiomer contained in the I(-)C(-) salt is analyzed using the process described in Example 1.1. The solid obtained shows a 99.5/0.5 ratio of the R(-)-I/S(+)-I enantiomers, which indicates a 99% enantiomeric excess for R(-)-I. [0086] The precipitated and dried salt is resuspended with stirring in 680 ml of ethyl acetate and 255 ml of 7% NaHCO3 solution, and is heated to 40-45 C., until obtaining a solution. The phases are separated and the organic phase is washed again two times with 170 ml of water, and then, a concentrated hydrochloric acid solution is added, adjusting the pH between 5 and 5.5. The solvent is partially distilled under reduced pressure, to half the volume, and is left to cool, the product precipitating as R(-)-I.HCl. Once dried, the collected product weighs 11.5 g (0.025 moles), an overall yield of 22% being obtained. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
85.65 - 89.67% | In water; isopropyl alcohol; at 0 - 4℃; for 1.5h;Heating / reflux;Product distribution / selectivity; | EXAMPLE 5:Preparation of Enantioraerically Enriched(R)-5-(2-aminopropyl)-2-methoxybenzenesu]fonamideThe enantiomeric enrichment of (R)-5-(2-aminopropyl)-2- methoxybenzenesulfonamide (reactant- V) is provided according to this example. In a round bottomed flask 20.88 g of (R)-5-(2-aminopropyl)-2-methoxybenzene-sulfonamide (85.46 mmol, e.e. 96.4% by HPLC method 2), 19.85 g of (lR)-(-)-10-camrhohorsulfonic acid (85.46 mmol), 310.86 g of isopropanol (396 mL) and 26,43 mL of water were charged. The resulting mixture was heated to reflux and was stirred for 30 minutes at this temperature; in this way, a yellowish homogeneous solution was obtained. This solution was cooled down to 2 +/- 20C and aged for 60 minutes. Then the off-white solid thus obtained was filtered under vacuum to yield 46.15 g of a wet solid (loss on drying: 24.4%, which corresponds to 34.88 g of dry material; Yield: 85.65%). EPO <DP n="21"/>To the above obtained solid, 617.01 g of isopropanol and 26.19 mL of water were added, and the mixture was heated to reflux and was stirred for 10 minutes at this temperature. The thick suspension thus obtained was cooled down to 2 +/- 20C, aged for 60 minutes and the resulting off-white solid was filtered under vacuum to yield 38.44 g of a wet solid (loss on drying: 10.43%, which corresponds to 34.43 g of dry material; Yield: 98.71%).To the solid thus obtained, 207 mL of water were added and the mixture was stirred for 30 minutes at 20-250C; in this way, a yellowish homogeneous solution was obtained. Then 25.06 mL of aqueous ammonia were added to the solution to adjust the pH at 10.18, with continuous stirring and keeping the temperature at about 250C, and a white solid was obtained. The mixture was concentrated by distillation under vacuum until 69.28 mL of water were distilled and a white solid precipitated out. Then 17.64 mL of aqueous ammonia at 250C were added to adjust the pH at 10.07. The obtained mixture was cooled down to 2 +/- 20C and aged for 60 minutes. The off-white solid thus obtained was filtered under vacuum and dried under vacuum at 6O0C to yield 14.65 g of (R)-5-(2-aminopropyl)-2-methoxybenzene-sulfonamide. (Yield: 82.06%, overall yield 69.4%, e.e. 100.0% by HPLC method 2) EXAMPLE 6:Preparation of Enantiomerically Enriched(R)-5-(2-aminopropyI)-2-niethoxybenzenesulfonamideThe enantiomeric enrichment of (R)-5-(2-aminopropyl)-2- methoxybenzenesulfonamide (reactant-V) is provided according to this example. In a round bottomed flask 41.76 g of (R)-5-(2-aminopropyl)-2-methoxybenzene-sulfonamide (107.9 mmol, e.e. 96.4% by HPLC method 2), 170.7 g of (lR)-(-)-10-camphorsulfonic acid (107.9 mmol), 621.7 g of isopropanol (792 mL) and 53 mL of water were charged. The resulting mixture was heated to reflux and was stirred for 30 minutes at this temperature; in this way, a yellowish homogeneous solution was obtained. This solution was cooled down to 2 +/- 20C and aged for 60 minutes. Then the off-white solid thus obtained was filtered under vacuum to yield 97.44 g of a wet solid (loss on drying: 25.0%, which corresponds to 73.05 g of dry material; Yield: 89.67%). EPO <DP n="22"/>To the above obtained solid, 1212 g of isopropanol (1544 mL) and 52 mL of water were added, and the mixture was heated to reflux and was stirred for 10 minutes at this temperature. The thick suspension thus obtained was cooled down to 2 +/- 20C, aged for 60 minutes and the resulting off-white solid was filtered under vacuum to yield 78,97 g of a wet solid (loss on drying: 25.6%, which corresponds to 58.72 g of dry material; Yield: 81.36%).To the solid thus obtained, 352 mL of water were added and the mixture was stirred for 30 minutes at 20-250C; in this way, a yellowish homogeneous solution was obtained. Then 42 mL of aqueous ammonia were added to the solution to adjust the pH at 9.89, with continuous stirring and keeping the temperature at about 25C, and a white solid was obtained. The mixture was concentrated by distillation under vacuum until 166 mL of water were collected and a white solid precipitated out. Then 14 mL of aqueous ammonia at 250C were added to adjust the pH at 9.97. The obtained mixture was cooled down to 2 +/- 20C and aged for 60 minutes. The off-white solid thus obtained was filtered under vacuum to yield 28.72 g of a wet solid (loss on drying: 12.55%, which corresponds to 25.15 g of dry material; Yield: 83.57%, overall yield 61.0%, e.e. 99.44% by HPLC method2).To the solid thus obtained, 314.7 g of isopropanol (401 mL) were added and the mixture was heated to reflux and was stirred for 30 minutes at this temperature. The solution was concentrated by distillation under atmospheric pressure until 165 g of isopropanol (211 ml) were collected and a white solid precipitated out. The mixture was cooled down to 2 +/- 20C and aged for 60 minutes. The off-white solid thus obtained was filtered under vacuum and dried under vacuum at 6O0C to yield 20.98 g of (R)-5-(2-aminopropyl)-2-methoxybenzene- sulfonamide. (Yield... |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
78.5% | Stage #1: (R)-10-camphorsulfonic acid; imatinib In methanol at 20℃; for 1h; Activated carbon; Stage #2: In isopropyl alcohol at 20℃; for 1h; | 3 Example 3 : Preparation of imatinib L-(-)-camphorsulphonic acid salt[42] 5 g of4-[(4-methyl-l-piperazinyl)methyl]-N-[4-methyl-3-[[4-(3-pyridyl)-2-pyrimidinyl]amin o]phenyl]-benzamide was added to 20 ml of methanol. While stirring, 2.4 g of L- (-)-camphorsulphonic acid and 0.1 g of activated carbon were slowly added thereto, and further stirred at room temperature for 1 hr. The solution was filtered, washed with 5 ml of methanol, and then distilled off under reduced pressure. Then, 50 ml of iso- propanol was added thereto, and stirred at room temperature for 1 hr. The solid mixture was filtered and washed with 10 ml of isopropanol, and then dried under reduced pressure to give 5.8 g of solid (78.5%).[43] Melting point (m.p.): 135-1360C |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In methanol; at 15 - 55℃; for 2.16667 - 3.25h; | Example 1 :Preparation of (2R,3S)-2- (2,4- difluoro phenyl )-3- (5- fluoro pyrimidin -4-yl )-l- (1H-1,2,4- triazol- 1 - yl) butan-2-ol-R (-) - 10-camphor sulfonate salt.; 250 gm of (2R,3S)-2- (2,4-difluoro phenyl) -3- (5-fluoro pyrimidin -4-yl) -1- (lH-l,2,4-triazol-l- yl) butane -2-ol was charged into a flask having 1.5 Lt of acetone 165 gm of R-(-) -10- camphor sulfonic dissolved in 500 ml of methanol was added and heated to about 50 - 55 C maintained for 10-15 min at 50 -55 C. the reaction mass was cooled to 15 -20 C and maintained for 2-3 hr. The separated solid was filtered and washed with 25 ml of acetone. Solid was dried filtered under vacuum of about 650 mm/Hg for about 8 hrs to yield 160 gm of the title compound. Further purification in acetone and methanol mixture (3:1) and heated to 50-55 C and maintained for 10-15 min. Then the reaction mass was cooled to 20-25 C and maintained for over night. The solid separated was filtered and washed with 25 ml of acetone. The obtained solid was dried at70 -75 C for about 10 hi- to yield 130 gm of title compound as a pure crystalline solid. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
75% | Preparation of S-(+)-Clopidogrel Camphor sulfonic acid salt [F]52.2 gm of 4, 5, 6, 7-tetrahydrothieno [3, 2, c] pyridine [D], 90 gm alpha bromo o-chloro phenyl acetic acid methyl ester [B] ,triethyl amine (44.6 gm) and toluene (270 ml) were charged in a 2 liter round bottom flask at 25-30 C and the reaction mixture was heated to reflux. The reflux was maintained for 3 hours. Water (150 ml) was added to the <n="12"/>reaction mixture at 25-30 0C. Separate organic (toluene) and aqueous layers. Water (90 ml) was added to the toluene layer followed by the addition of aqueous hydrochloric acid (4.8 ml). Separate organic (toluene) and aqueous layers. Wash organic layer (toluene) with 10% solution of sodium bicarbonate. The toluene layer was distilled under vacuum to get racemic clopidogrel base (E) as oily residue (102 gm). Leavo- camphor-10- sulfonic acid (34.4 gm) and acetone (396 ml) was charged in the 2 liter round bottom flask containing clopidogrel base at 25-30 C. The reaction mixture was heated to 50-55 C under stirring and maintained for 1 hour. The reaction mixture was cooled to 25-30 C under stirring and S-(+) clopidogrel camphor sulphonic acid salt (0.1 gm) was added as a seed. This reaction mixture was stirred at 25-30 C for 24 hours and filtered at 25-30 C. S-(+)-clopidogrel camphor sulfonic acid salt [F] obtained was washed twice with Acetone (50ml) and was dried in the oven at 50-55 C. S-(+)-clopidogrel camphor sulfonic acid salt [F] may be purified if required in acetone or in a mixture of acetone and IPA to obtain the desired enantiomeric purity. Yield: 72 to 82 gms % Yield: 65-75 |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
19% | In methanol; at 20℃; for 1h; | 500 mg (2.920 mmoles) of <strong>[136236-51-6]rasagiline</strong> base and 677 mg (2.915 mmoles) of (li?)-10-camphorsulfonic acid are dissolved in 1.0 ml of methanol. The solution is stirred for an hour, evaporated to dryness in vacuo and the residue is treated with diisopropyl ether. The solid product is filtered off and washed with diisopropyl ether. Thus 1.051 g of a beige coloured crude salt is obtained which is crystallized from a mixture of hot isopropyl-alkohol and diisopropyl ether. The suspension thus formed is cooled with an ice-water bath, the precipitated crystals are filtered and finally washed with cold diisopropyl ether.Yield 219 mg (19 %), off-white crystals.Mp,: 140-142C.Elementary analysis for the Formula: C22H29N04S (403.54):Calculated [%] C: 65.48 H: 7.24 N: 3.47 S: 7.95 O: 15.86 Found [%] C: 65.23 H: 7.00 N: 3.34 S: 8.14IR (KBr): 3442, 3228, 2958, 2806, 1745, 1482, 1230, 1 167,1041 cm"1.1H-NMR (DMSO-i¾, 400 MHz) delta 9.47 (s, 2H), 7.61 (d, 1H, J = 7.6Hz), 7.38 (m, 1H), 7.37 (m, 1H), 7.31 (m, 1H), 4.82 (dd, 1H, J = 7.7, 4.3 Hz), 4.02 (dd, 1H, J = 17.6, 2.6 Hz), 3.98 (dd, 1H, J = 17.6, 2.5 Hz), 3.76 (t, 1H, J = 2.5 Hz), 3.12 (m, 1H), 2.90 (m, 1H), 2.89 (d, 1H, J= 14.8 Hz), 2.67 (m, 1H), 2.44 (m, 1H), 2.39 (d, 1H, J = 14.8 Hz), 2.23 (m, 1H), 2.21 (m, 1H), 1.94 (t, 1H, J = 4.6 Hz), 1.85 (m, 1H), 1.79 (d, 1H, J = 18.1 Hz), 1.29 (m, 1H), 1.27 (m, 1H), 1.05 (s, 3H), 0.74 (s, 3H) ppm.HPLC purity: >99.8 %[a] 22D = +l l,l (c=l; EtOH) |
In n-heptane; isopropyl alcohol; | Example 15; (Rasagiline (-)-camphor-10-sulfonate) Rasagiline base (0.57g) was dissolved in 2-propanol (10 ml) and was combined with solution of (-)-camphor-10-sulfonic acid (0.77 g) in 2-propanol (5 ml). To this combined solution 20 ml of heptane was slowly added, and left to evaporate slowly. After several hours crystals of <strong>[136236-51-6]rasagiline</strong> (-)-camphor-10-sulfonate formed. | |
In isopropyl alcohol; | Rasagiline base (0.57g) was dissolved in 2-propanol (10 ml) and was combined with solution of (-)-camphor-I O-sulfonic acid (0.77 g) in 2-propanol (5 ml). To this combined solution 20 ml of heptane was slowly added, and left to evaporate slowly. After several hours crystals of <strong>[136236-51-6]rasagiline</strong> (-)-camphor-I O-sulfonate formed. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In water; isopropyl alcohol; at 70℃; for 0.166667h; | Example 21 : Preparation of an R-Camsylate Salt of Compound , R-Camsylate Polymorph Form A.A slurry of Compound (1 .5 g) was prepared in isopropyl alcohohwater (25 ml 40:60 % v/v). R-camphor sulfonic acid (1.3 g) was added, as a solution, in water (1 .5 ml_). The slurry was heated to 70 C over a 10 minute period. The resultant solution was cooled to 10 C over a 10 minute period. Solid crystallized after holding this solution at a temperature of 10 C. This resulted in the formation of a slurry. This slurry was granulated for a total of 4 hours. The crystals were filtered and washed with water and then dried overnight at 50 C providing a pale yellow powder. | |
0.25 g | In ethanol; at 75 - 85℃; for 3h; | 0.2 g of <strong>[283173-50-2]Rucaparib</strong> Form M2 was dissolved in 4 mL of ethanol at 80±5C. To the clear solution was added (S)-Camphor sulfonic acid solution [dissolved (S)-camphor sulfonic acid (0.l4g) in ethanol (lmL)] slowly at 80±5C for 5-10 min and maintained under stirring for 3h. The reaction mass was cooled to 25±5C and further stirred for 12 h. The reaction mass was filtered and dried under vacuum at 50C for 3h. The product obtained was identified as <strong>[283173-50-2]Rucaparib</strong> S- Camsylate Form Ml. (0130) Yield: 0.25 g |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
7 g | In ethyl acetate; acetone at 25 - 30℃; for 12h; | 5 Preparation of camphor sulphonate salt of Donepezil Donepezil base (5 gm) and ethyl acetate (90 ml) were taken into the round bottom flask and stirred for 10- 15 minutes at 25-30°C to get clear solution. L (-) camphor sulfonic acid solution (5 gm L (-) camphor sulfonic acid in 45 ml acetone) was added to the reaction mass at 25-30°C. The reaction mass was stirred at 25-30°C for 12 hours and solvent distilled under vacuum at 50-55°C to obtain camphor sulfonate salt of donepezil. Dry weight: 7.0 gm |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In isopropyl alcohol; for 0.5h;Reflux; | Compound B1 (1 eq.) dissolved in IPA, refluxed for 30 min., acid (1eq.) in IPA was added, the clear solution not obtained, the residue was evaporated completely and was washed with water. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
5.1 g | In methanol; at 25 - 30℃; for 5.16h; | Preparation of <strong>[106266-06-2]Risperidone</strong> Camphor Sulfonate 15 ml methanol and 2.8 gm of L (-) camphor sulfonic acid were charged in flask. The reaction mixture was stirred for 10 minutes at 25-30 C. to obtain clear solution. 5 gm <strong>[106266-06-2]Risperidone</strong> solution in 80 ml methanol was added to the reaction mixture within 15-20 minutes at 25-30 C. The reaction mixture was stirred for 5 hours and was distilled out completely under vacuum at 50-55 C. 20 ml of acetone was added further and stirred for 10 minutes at 40-45 C. The reaction mixture was cooled to -5 to -10 C. and stirred for 4 hours. The solid was filtered off, washed with 5 ml acetone and dried in vacuo at 50-55 C. for 12 hours. Dry weight: 5.1 gm DSC: 120.4 C. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With barium(II) perchlorate In methanol Resolution of racemate; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Preparation of Voriconazole Camphorsulfonate (wet) from Hydrochloride Salt of (2R,3S/2S,3R)-3-(4-chloro-5-fluoropyrimidin-6-yl)-2-(2,4-difluorophenyl)-1-(1H-1,2,4-triazol-1-yl)butan-2-ol. Hydrochloride salt of (2R,3S/2S,3R)-3-(4-chloro-5-fluoropyrimidin-6-yl)-2-(2,4-difluorophenyl)-1-(1H-1,2,4-triazol-1-yl)butan-2-ol (180 gm) obtained from Step III of Example 1 or Example 2 or Example 3 was added to methanol (720 mL) at 20 C.-25 C. followed by pH adjustment (8.0-9.0) with 40% w/v aqueous sodium hydroxide solution (50 mL) under nitrogen blanketing. To this reaction mixture, ammonium formate (108.2 gm) was added followed by addition of wet palladium/carbon [Pd/C (2.5% w/w dry, 18 gm)] treated with de-ionized water. The reaction mixture was further heated and stirred at 55 C.-60 C. followed by cooling of the mixture to 30 C.-35 C. The reaction mixture was filtered through hyflobed and washed with methanol (360 mL) first and then with a mixture of de-ionized water (1800 mL) and dichloromethane (900 mL) at 15 C.-20 C. followed by stirring. To the organic layer, de-ionized water (360 mL) was added followed by pH adjustment with 2N hydrochloric acid solution (6 mL) at the same temperature. The solvent was recovered under reduced pressure at 40 C.-45 C. to give residual solid. To the residue acetone (2700 mL) was added followed by addition of the methanolic solution of (1R)-(-)-10-camphorsulfonic acid (99.5 gm in 900 mL methanol) at 40 C.-45 C. Seed of voriconazole camphorsulfonate (0.18 gm) was added to the reaction mixture and the mixture stirred at 40 C.-45 C. for 60 minutes. The slurry so obtained was cooled to 30 C.-35 C. followed by further cooling to 20 C.-25 C. The mixture was stirred for 10-12 hours at 20 C.-25 C. followed by filtration and washing with acetone (180 mL) to give wet voriconazole camphorsulfonate. Wet wt: 91 gm. Voriconazole camphorsulfonate (wet) (entire quantity from Step 4A of Example 4) was added to a stirred mixture of de-ionized water (360 mL) and dichloromethane (360 mL) at 15 C.-25 C. followed by pH adjustment of the mixture to pH 10-11 with 40% w/v aqueous sodium hydroxide solution (16.2 mL). The organic layer was washed with de-ionized water (360 mL) followed by filtration of organic layer through 0.45 micron filter. The filtered layer was further washed with dichloromethane (90 mL) and solvent was recovered under reduced pressure (50-500 torr) at 35 C.-45 C. to give a residual solid. Isopropyl alcohol (450 mL) was added to the residue followed by heating and stirring of the mixture at 60 C.-70 C. until the mixture was dissolved, followed by recovery of isopropyl alcohol under reduced pressure (50-500 torr) at 50 C.-60 C. to obtain a residual volume of 270 mL. The concentrated solution so obtained was heated to 60 C.-70 C. followed by cooling of the solution to 45 C.-50 C. The solution was further cooled to 5 C.-10 C. followed by stirring for 60 minutes at the same temperature. The solid obtained was filtered and washed with isopropyl alcohol (135 mL) followed by drying of the solid under reduced pressure at 50 C.-55 C. until constant weight. %Yield: 42.8% |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
75% | In acetone at 20℃; for 12h; Resolution of racemate; | Preparation of (S)-(C)-Clopidogrel Camphorsulfonate Salt The racemic clopidogrel bisulfate2(1.5 g, 3.75 mmol) andLCSA (0.88 g, 3.75 mmol) were dissolved in acetone andstirred at room temperature for 12 h. The formed precipitatewasfiltered, washed and dried to give a white solid as a (S)-clopidogrel camphor sulfonate salt (0.96 g, 75% yield),[a]DDC25 (cD1.68% in CH3OH); IR:v(KBr, cm-1) 3454(N-H stretch), 2975, 1756 (C DO stretch), 1735, (CDOstretch), 1630, 1506, 1473, 1439, 1263, 1234, 1157, 1030, 753,724, 701. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
88 g | In butanone; at 20℃; for 1h; | 1000ml three necked flask, <strong>[14813-01-5]N-benzyl-<strong>[14813-01-5]3-hydroxypiperidine</strong></strong> (95.6 g, 0.5 mol), 2-Butanone (478 ml) was added dropwise a solution of L-CSA (58 g, 0.25 mol) in 290 ml of 2-butanone at room temperature Stirring for 1 hour, precipitation of solid appeared, 0 heat 2 hours, filtration, 2-butanone 30ml washing,Dried to obtain 88 g of (S) -<strong>[14813-01-5]1-benzyl-<strong>[14813-01-5]3-hydroxypiperidine</strong></strong> camphorsulfonate. (Ee: 93%) (theory: 105.9 g). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
108 g | In butanone; at 20℃; for 1h; | 1000ml three necked flask n-Benzyl-<strong>[14813-01-5]3-hydroxypiperidine</strong> (95.6 g, 0.5 mol) was added,2-butanone 478 ml of a solution of L-CSA (69.6 g, 0.3 mol) in 290 ml of 2-butanone was stirred at room temperature for 1 hour, and the precipitated solid appeared, kept at 0 C for 2 hours, filtered, washed with 2-butanone 30 ml, (S) -<strong>[14813-01-5]1-benzyl-<strong>[14813-01-5]3-hydroxypiperidine</strong></strong> camphorsulfonate. (Ee: 75%)(Theory: 105.9G). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
86% | Assemble a 2000 mL 3-neck RBF with an addition funnel, nitrogen inlet and a thermometer adapter. Purge the vessel with nitrogen and add (3R)-butane-1,3-diol (25 g, 277.4 mmol), DIPEA (127 ml, 731 mmol) and ACN (556 ml). Cool to -30 C. Add trifluoromethanesulfonic anhydride (101 mL, 601 mmol) dropwise over 3 h such that the internal temperature is maintained between -35 and -30 C. After the completion of the addition, stir for 10 min at -35 to -30 C. Add trifluoromethanesulfonic anhydride (1.9 mL, 11 mmol) dropwise over 5 min such that the internal temperature is maintained between -35 and -30 C. After the completion of the addition, stir for 10 min at -35 to -30 C. Add DIPEA (127 mL, 731 mmol) dropwise over 15 min such that the internal temperature is maintained between -35 and -30 C. After the completion of the addition, stir for 10 min at -35 to -30 C. In a separate flask under nitrogen, dissolve aminodiphenylmethane (48.0 mL, 270 mmol) in ACN (49 mL, 935 mmol) and transfer the resulting solution to the addition funnel. Add the amine solution to the cold triflate dropwise over 40 min such that the internal temperature is maintained between -20 to -35 C. After the completion of the addition, stir for 30 min at -35 to -30 C. Transfer the reaction to a water bath and allow it to slowly warm over 30 min. Remove the bath and allow the reaction to warm to RT over 30 min. Transfer the vessel to a heating mantle and warm the reaction to 45 C. for 30 min, then cool to RT. Pour the resulting mixture into 1200 mL of water and extract with toluene (400 mL×3). Combine the extracts, wash with water, sat. aq. NaCl solution, dry over anhydrous Na2SO4, filter and concentrate on a rotary evaporator. Dry the material under vacuum overnight. Dissolve the residue in DCM (400 mL). Prepare a silica pad on a fritted funnel and equilibrate it with 1:1 heptane/EtOAc. Load the product solution onto the silica pad and wash with 1600 mL of 1:1 heptane/EtOAc. Concentrate the filtrate to give a red oil. Dissolve the oil in MeOH (250 mL) and place the flask in a water bath (10 C.). Add L(-)-camphorsulfonic acid (61.6 g, 265 mmol) portion-wise keeping the internal temperature below 20 C. Stir the resulting mixture for 15 min and then concentrate on a rotary evaporator to give a brown foam. Dry the foam on a vacuum pump for 2 h. Dissolve the foam in 130 mL of DCM. Attach an addition funnel to the flask. Use the funnel to slowly add 1100 mL of EtOAc to the stirring solution. Transfer the resulting mixture to a 4000 mL beaker and stir open to the atmosphere overnight. Cool the beaker in an ice bath for 10 min. Collect the precipitate in a fritted funnel by vacuum filtration washing with a minimal amount of ice-cold EtOAc. Dry the solid on the frit for 2 h. Dissolve the resulting white solid in a minimal amount of DCM, transfer to a 2000 mL beaker and then dilute slowly with EtOAc until the clear solution starts to become cloudy. Stir the suspension for 4 h while open to the atmosphere. Collect the solids by vacuum filtration using a fritted funnel and dry on the frit overnight to give the title compound (111.8 g, 238.06 mmol, 86% Yield) as a white solid. 1H NMR (400 MHz, d6-DMSO): 10.54-10.47 (m, 1H), 7.61 (d, J=7.3 Hz, 5H), 7.47-7.37 (m, 7H), 5.85 (d, J=10.3 Hz, 1H), 4.68-4.61 (m, 1H), 3.91-3.83 (m, 2H), 3.37 (s, 8H), 2.99 (d, J=14.6 Hz, 1H), 2.77-2.68 (m, 1H), 2.51-2.44 (m, 4H), 2.30-2.16 (m, 2H), 1.91-1.81 (m, 2H), 1.42-1.28 (m, 3H), 1.08 (s, 3H), 1.01 (d, J=6.6 Hz, 3H), 0.77 (s, 4H); >98% ee [HPLC: Chiralcel OJ (10 cm×4.6 mm, 5 [mum), 5 mL/min, 40 C. isocratic 10% EtOH (0.2% iPrNH2)/CO2]. | |
65% | A solution of R-(-)-1,3-butanediol (20.0 g, 222 mmol) and DIPEA (101.5 mL, 585.0 mmol) in acetonitrile (444 mL) was cooled to -30 C. and treated with trifluoromethanesulfonic anhydride (81.2 mL, 480 mmol) dropwise via addition funnel over 90 min, maintaining the internal reaction temperature between -30 and -35 C. After the addition was complete, the reaction mixture was stirred for 10 min at -30 C. and then treated with additional trifluoromethanesulfonic anhydride (1.5 mL) dropwise and stirred at -30 C. for an additional 15 min. The reaction mixture was then treated with additional DIPEA (101.5 mL, 585.0 mmol) over the course of 15 min while maintaining the internal temperature at -30 C. After an additional 10 min at -30 C. the reaction mixture was treated with a solution of benzhydrylamine (38 mL) in acetonitrile (40 mL) dropwise over 30 min via an addition funnel, maintaining the internal reaction temperature below -30 C. The reaction mixture was stirred at -30 C. for 20 min then placed in an ice water bath for 30 min. The reaction was then stirred at rt for 30 min, followed by heating at 45 C. for 30 min. The reaction mixture was cooled to rt, poured into deionized water (900 mL) and extracted with toluene (1 L). The aqueous phase was back-extracted with toluene (300 mL) and the combined organic layers were washed with water (2*250 mL), dried over Na2SO4, filtered and evaporated. The crude product was dissolved in DCM (300 mL) and loaded onto a plug of silica gel (300 mL SiO2, preflushed with 1:1 heptane/EtOAc). The plug was flushed with 1:1 heptane/EtOAc (1.2 L) and the filtrate was evaporated to give a red oil (50.2 g). The crude product was dissolved in methanol (200 mL), placed in a water bath at 10 C., and treated with [(1R,4S)-7,7-dimethyl-2-oxobicyclo[2.2.1]hept-1-yl]methanesulfonic acid (49 g) in batches over 5 minutes. The solution was stirred at rt for 2 h, the solvent was evaporated and the solids were dried under high vacuum for 15 h to give a solid (99.2 g). The solid was dissolved in DCM (100 mL) and stirred at rt for 10 min to give a dark solution. EtOAc (850 mL) was added slowly with stirring and solids precipitated from solution after ?5 min. The suspension was stirred at rt for 2 h, and the solids were collected by filtration and washed with EtOAc (50 mL). The solids were dissolved in DCM (100 mL) and EtOAc (700 mL) was added. The mixture was stirred at rt and solids immediately precipitated from solution. The suspension was stirred at rt for 15 h, then the solids were collected by filtration, washed with EtOAc (50 mL) and dried under reduced pressure to give the title compound (66.7 g, 65% yield) as a white solid. 1H NMR (500 MHz, CD3OD) delta: 7.54-7.59 (m, 4H), 7.43-7.53 (m, 6H), 5.67 (s, 1H), 4.69-4.76 (m, 1H), 3.97-4.02 (m, 2H), 3.36 (d, 1H), 2.81 (d, 1H), 2.70-2.75 (m, 1H), 2.58-2.64 (m, 1H), 2.31-2.39 (m, 2H), 2.03-2.09 (m, 2H), 1.91 (d, 1H), 1.62-1.66 (m, 1H), 1.41-1.47 (m, 1H), 1.16 (s, 3H), 1.11 (d, 3H), 0.88 (s, 3H); Elemental analysis: Calculated for C27H35NO4S: C=69.05%, H=7.51%, N=2.98%; Found: C=68.90%, H=7.59%, N=2.91%. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
40 g | Compound of Formula XII (50 g), acetonitrile (250 mL) and <strong>[434-76-4]2-amino-6-fluoro-benzoic acid</strong> (28.8 g) were charged in a reaction flask at 25-35C. To the reaction mass hexamethyldisilazane (5.4 g) and zinc chloride (68.9 g) were charged at 25-35C and stirred for 2 hrs at same temperature. Reaction mass was heated to 70-80C and stirred for 4 hrs at same temperature. After completion of the reaction, the reaction mass was allowed to cool to 25-35C and quenched in to water (1.25 lit). Precipitated solid was filtered and the obtained solid was dissolved in a mixture of methylene chloride (3 lit) and trifluoro acetic acid (50 mL) at 25-35C. To the reaction mass water (250 lit) was added at 25-35C and pH was adjusted to 7-7.5 with sodium bicarbonate solution at same temperature. Then the organic and aqueous layers were separated distilled completely under vacuum at below 40C to obtain a residue. The obtained residue was dissolved in acetonitrile (100 mL) at 25-35C and R (-)-camphor sulfonic acid (43 g) was added and stirred for 3 hrs at same temperature. Precipitated solid compound was filtered and washed with acetonitrile (25 mL) and dried to obtain idelalisib camphor sulfonate salt. Yield: 40g. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
84.8% | Stage #1: ethyl 4-oxocyclohexane-1-carboxylate; (R)-10-camphorsulfonic acid In ethylene glycol; toluene at 60℃; for 4h; Inert atmosphere; Dean-Stark; Large scale; Stage #2: 4-Chloro-6-fluoroquinoline With sodium hexamethyldisilazane In tetrahydrofuran; N,N-dimethyl-formamide; toluene at -20℃; for 3h; Large scale; Stage #3: In ethylene glycol Large scale; | 1; 1A Example 1A A reactor was charged with ethyl 4-oxocyclohexane-1-carboxylate 12 (129 kg, 1.4 equiv), toluene (1122 kg) ethylene glycol(93 kg, 2.1 equiv), and (1R)-(-)-10- Camphorsulfonic Acid (CSA) (1.6 kg, 0.010 equiv). The mixture was heated to reflux (60 °C) under vacuum under Dean-Stark conditions. The mixture was held for 4 h then cooled to 25 °C. The organic stream was washed with 5% aqueous solution of NaHCO3 (2 x 325 kg). The organic layer was washed with water (309 kg) and the organic layer was concentrated to 650 L. The mixture was charged to a solution of 4-chloro-6-fluoroquinoline (129 kg, 1.0 equiv) and DMF (611 kg). The solution was agitated until homogenous and cooled to -20 °C. To this solution was charged 40 wt% NaHMDS solution in THF (719 kg) while maintaining the temperature |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
79.8% | In ethanol; at 20 - 50℃; | <strong>[284461-73-0]4-{4-[([4-chloro-3-(trifluoromethyl)phenyl]amino}carbonyl)amino]phenoxy}-N-methylpyridine-2-carboxamide</strong> (10.0 g, 21.51 mmol), and ethanol (100 mL) were added to the reactor. (-)-10-camposulfonic acid (5.25 g, 22.59 mmol) was added, followed by stirring at room temperature for 30 minutes. The reaction solution was stirred at 50 C for 30 minutes or more, cooled to 20 to 30 C, and stirred for 2 hours or more. After filtering the reaction mixture under reduced pressure, the wet cake was washed with ethanol (10 mL) and the obtained solid was vacuum dried at 50 to 60 C to obtain 9.98 g of the compound prepared in Example 4 (Yield: 79.8%). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
92% | In methanol; isopropyl alcohol at 0℃; for 1.5h; | 2.2. Synthesis of 4-vinyl benzylamine salts General procedure: In round-bottom flask (100 mL), 4-vinyl benzylamine (0.80 g,6.3 mmol) was dissolved in 20 mL of methanol, and then 15 mL of isopropanolsolution containing β-naphthalene sulfonic acid 1a (1.31 g,6.3 mmol) was added dropwise (about 1.5 h) at 0 °C. The precipitatewas filtered and dried to afford white 4-vinyl benzylamine naphthalenesulfonate 1a (2.0 g, 95 %).When sulfonic acid 1a was replaced by camphorsulfonic acid 1band adamantane formic acid 1c, yellow sulfonic amine salt 1b (2.1 g,92 %) and white carboxylic acid amine salt 1c (1.6 g, 80 %) were alsoprepared according to the above-mentioned procedure. |
Tags: 35963-20-3 synthesis path| 35963-20-3 SDS| 35963-20-3 COA| 35963-20-3 purity| 35963-20-3 application| 35963-20-3 NMR| 35963-20-3 COA| 35963-20-3 structure
A644249[ 3144-16-9 ]
((1S,4R)-7,7-Dimethyl-2-oxobicyclo[2.2.1]heptan-1-yl)methanesulfonic acid
Reason: Optical isomers
[ 209736-59-4 ]
((1S,3S,4S)-3-Bromo-7,7-dimethyl-2-oxobicyclo[2.2.1]heptan-1-yl)methanesulfonic acid hydrate
Similarity: 0.78
[ 14575-84-9 ]
Ammonium ((1R,3S,4S,7R)-3-bromo-1,7-dimethyl-2-oxobicyclo[2.2.1]heptan-7-yl)methanesulfonate
Similarity: 0.75
[ 55870-50-3 ]
Ammonium ((1S,3R,4R,7S)-3-bromo-1,7-dimethyl-2-oxobicyclo[2.2.1]heptan-7-yl)methanesulfonate
Similarity: 0.75
[ 209736-59-4 ]
((1S,3S,4S)-3-Bromo-7,7-dimethyl-2-oxobicyclo[2.2.1]heptan-1-yl)methanesulfonic acid hydrate
Similarity: 0.78
[ 1588441-14-8 ]
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[ 26978-64-3 ]
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[ 3687-18-1 ]
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[ 209736-59-4 ]
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Similarity: 0.78
[ 14575-84-9 ]
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[ 55870-50-3 ]
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[ 63738-92-1 ]
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P413 | |
P420 | Store away from other materials. |
P422 | |
P402 + P404 | Store in a dry place. Store in a closed container. |
P403 + P233 | Store in a well-ventilated place. Keep container tightly closed. |
P403 + P235 | Store in a well-ventilated place. Keep cool. |
P410 + P403 | Protect from sunlight. Store in a well-ventilated place. |
P410 + P412 | Protect from sunlight. Do not expose to temperatures exceeding 50 oC/122oF. |
P411 + P235 | Keep cool. |
Disposal | |
Code | Phrase |
P501 | Dispose of contents/container to ... |
P502 | Refer to manufacturer/supplier for information on recovery/recycling |
Physical hazards | |
Code | Phrase |
H200 | Unstable explosive |
H201 | Explosive; mass explosion hazard |
H202 | Explosive; severe projection hazard |
H203 | Explosive; fire, blast or projection hazard |
H204 | Fire or projection hazard |
H205 | May mass explode in fire |
H220 | Extremely flammable gas |
H221 | Flammable gas |
H222 | Extremely flammable aerosol |
H223 | Flammable aerosol |
H224 | Extremely flammable liquid and vapour |
H225 | Highly flammable liquid and vapour |
H226 | Flammable liquid and vapour |
H227 | Combustible liquid |
H228 | Flammable solid |
H229 | Pressurized container: may burst if heated |
H230 | May react explosively even in the absence of air |
H231 | May react explosively even in the absence of air at elevated pressure and/or temperature |
H240 | Heating may cause an explosion |
H241 | Heating may cause a fire or explosion |
H242 | Heating may cause a fire |
H250 | Catches fire spontaneously if exposed to air |
H251 | Self-heating; may catch fire |
H252 | Self-heating in large quantities; may catch fire |
H260 | In contact with water releases flammable gases which may ignite spontaneously |
H261 | In contact with water releases flammable gas |
H270 | May cause or intensify fire; oxidizer |
H271 | May cause fire or explosion; strong oxidizer |
H272 | May intensify fire; oxidizer |
H280 | Contains gas under pressure; may explode if heated |
H281 | Contains refrigerated gas; may cause cryogenic burns or injury |
H290 | May be corrosive to metals |
Health hazards | |
Code | Phrase |
H300 | Fatal if swallowed |
H301 | Toxic if swallowed |
H302 | Harmful if swallowed |
H303 | May be harmful if swallowed |
H304 | May be fatal if swallowed and enters airways |
H305 | May be harmful if swallowed and enters airways |
H310 | Fatal in contact with skin |
H311 | Toxic in contact with skin |
H312 | Harmful in contact with skin |
H313 | May be harmful in contact with skin |
H314 | Causes severe skin burns and eye damage |
H315 | Causes skin irritation |
H316 | Causes mild skin irritation |
H317 | May cause an allergic skin reaction |
H318 | Causes serious eye damage |
H319 | Causes serious eye irritation |
H320 | Causes eye irritation |
H330 | Fatal if inhaled |
H331 | Toxic if inhaled |
H332 | Harmful if inhaled |
H333 | May be harmful if inhaled |
H334 | May cause allergy or asthma symptoms or breathing difficulties if inhaled |
H335 | May cause respiratory irritation |
H336 | May cause drowsiness or dizziness |
H340 | May cause genetic defects |
H341 | Suspected of causing genetic defects |
H350 | May cause cancer |
H351 | Suspected of causing cancer |
H360 | May damage fertility or the unborn child |
H361 | Suspected of damaging fertility or the unborn child |
H361d | Suspected of damaging the unborn child |
H362 | May cause harm to breast-fed children |
H370 | Causes damage to organs |
H371 | May cause damage to organs |
H372 | Causes damage to organs through prolonged or repeated exposure |
H373 | May cause damage to organs through prolonged or repeated exposure |
Environmental hazards | |
Code | Phrase |
H400 | Very toxic to aquatic life |
H401 | Toxic to aquatic life |
H402 | Harmful to aquatic life |
H410 | Very toxic to aquatic life with long-lasting effects |
H411 | Toxic to aquatic life with long-lasting effects |
H412 | Harmful to aquatic life with long-lasting effects |
H413 | May cause long-lasting harmful effects to aquatic life |
H420 | Harms public health and the environment by destroying ozone in the upper atmosphere |
Sorry,this product has been discontinued.
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