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[ CAS No. 2495-39-8 ]

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Chemical Structure| 2495-39-8
Chemical Structure| 2495-39-8
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CAS No. :2495-39-8 MDL No. :MFCD00051416
Formula : C3H5NaO3S Boiling Point : -
Linear Structure Formula :- InChI Key :N/A
M.W :144.12 g/mol Pubchem ID :23690996
Synonyms :

Safety of [ 2495-39-8 ]

Signal Word:Warning Class:N/A
Precautionary Statements:P233-P260-P261-P264-P271-P280-P302+P352-P304-P304+P340-P305+P351+P338-P312-P321-P332+P313-P337+P313-P340-P362-P403-P403+P233-P405-P501 UN#:N/A
Hazard Statements:H315-H319-H335 Packing Group:N/A
GHS Pictogram:

Application In Synthesis of [ 2495-39-8 ]

  • Downstream synthetic route of [ 2495-39-8 ]

[ 2495-39-8 ] Synthesis Path-Downstream   1~14

  • 1
  • [ 2495-39-8 ]
  • [ 14418-84-9 ]
YieldReaction ConditionsOperation in experiment
With thionyl chloride; at 70℃; for 36h; A suspension of sodium allylsulfonate (2.0 g) in thionyl chloride (10.4 mL) was heated at 70C and stirred for 1.5 days. The insoluble material was removed by filtration, and the solvent of the filtrate was removed under reduced pressure. The obtained residue was dissolved in dry tetrahydrofuran (10 mL), and the solvent was removed under reduced pressure. The obtained residue was again dissolved in dry tetrahydrofuran (10 mL), and the solvent was removed under reduced pressure to give allylsulfonyl chloride (1.26 g). To a suspension ofN-benzyloxycarbonyl-1,2-diaminoethane hydrochloride (0.82 g) and triethylamine (0.63 g) in dichloromethane (5 mL) was added allylsulfonyl chloride (0.25 g) at room temperature, and the mixture was stirred overnight. The reaction was quenched by addition of water, and the organic layer of the resulting mixture was separated. The organic layer was washed with 1 mol/L hydrochloric acid, a saturated aqueous sodium hydrogen carbonate solution and brine successively, and dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure to giveN-(2-benzyloxycarbonylaminoethyl)allylsulfonamide (82 mg). This material was dissolved in acetonitrile (0.25 mL). To the solution were added 3-(2,3,4,6-tetra-O-acetyl-beta-D-glucopyranosyloxy)-4-[(4-bromophenyl)methyl]-5-isopropyl-1H-pyrazole (70 mg), triethylamine (57 mg), palladium acetate (II) (3 mg) and tris(2-methylphenyl)phosphine (7 mg), and the mixture was refluxed overnight under shading the light. The solvent was removed under reduced pressure, and the residue was dissolved in methanol (0.5 mL). To this solution was added 5 mol/L aqueous sodium hydroxide solution (0.25 mL), and the mixture was stirred at room temperature for 1 hour. The insoluble material was removed by filtration, and the filtrate was purified by preparative reverse phase column chromatography (Shiseido CAPCELL PAK UG120 ODS, 5 muL, 120A, 20x50mm, flow rate 30mL/minute linear gradient, water/methanol = 90/10 - 10/90) to give 4-({4-[(1E)-3-(2-benzyloxycarbonylaminoethylsulfamoyl)prop-1-enyl]phenyl}methyl)-3-(beta-D-glucopyranosyloxy)-5-isopropyl-1H-pyrazole (14 mg). This material was dissolved in methanol (0.5 mL). To the solution was added 10% palladium-carbon powder (5 mg), and the mixture was stirred at room temperature under a hydrogen atmosphere for 3 hours. The insoluble material was removed by filtration, and the solvent of the filtrate was removed under reduced pressure to give the title compound (10 mg).1H-NMR (CD3OD) delta ppm: 1.1-1.2 (6H, m), 2.0-2.1 (2H, m), 2.65-2.75 (4H, m), 2.85-2.95 (1H, m), 2.95-3.05 (4H, m), 3.25-3.45 (4H, m), 3.6-3.9 (4H, m), 5.0-5:1 (1H, m), 7.05-7.2 (4H, m)
2.95 g With thionyl chloride; In benzene; at 20 - 65℃; for 1h;Inert atmosphere; Preparation of prop-2-ene-1-sulfonyl chloride (22): In a flask was added sodium prop-2-ene-1-sulfonate (21, 4 g 27.75 mmol), followed by dropwise addition of thionyl chloride (10 mL, 137.09 mmol, 4.9 eq) at room temperature. The mixture was then stirred at 65 C. under nitrogen for 1 hrs. Due to stirring difficulty, benzene (5 mL) and thionyl chloride (2 mL) were added. The mixture was stirred at 65 C. under nitrogen, overnight. After the mixture was cooled to room temperature, TBME (30 mL) and sodium sulfate were added. The mixture was stirred for 30 min and filtered through a layer of silica gel. The filtrate was concentrated to give compound 22 as a pale brown liquid (2.95 g, 76 yield), which was used in next step without purification.
With oxalyl dichloride; N,N-dimethyl-formamide; at 0 - 20℃; To a stirred solution of sodium prop-2-ene-1-sulfonate (7 g, 48.61 mmol) in oxalyl chloride (70 mL), DMF (1.5 mL) was added at 0C and stirred at room temperature for 3 h. Progress of the reaction was monitored by TLC. After completion of the reaction, the reaction mixture was concentrated and the residue was trituration with ether to afford 10. Yield: 3.6 g, crude.
3.2 g With trichlorophosphate; In neat (no solvent); at 120℃; for 4h; A solution of sodium prop-2-ene-l -sulfonate 190 (15 g, 104.17 mmol) in POCl3 (100 mL) was stirred at 120 C for 4h. After completion of reaction, POCI3 was removed completely under reduced pressure. Residue was diluted with ethyl acetate (200 mL), organic layer was washed with water (100 mL x 3), dried over sodium sulphate and evaporated under reduced pressure to get crude prop-2-ene-l-sulfonyl chloride 191 (3.2 g, 22 %) as colorless liquid which was directly used as such for the next step. 1H NMR (400 MHz, DMSO-
With trichlorophosphate; at 0℃; for 5h;Reflux; Prop-2-ene-1-sulfonyl chloride (1) was prepared by ourmodification on the reported method28 as in the following: To a stirred solution of allyl bromide (12.10 g,0.1mol) in 100 mL distilled water was added Na2SO3 (15 g, 0.12mol). The reaction mixture was refluxed for 8hthen left to cool to room temperature. The reaction mixture was washed with Et2O several times and theaqueous layer was evaporated under reduced pressure. The crude product was washed with methanol,filtered off and left to dry to afford (10.2g, 0.07 mol, 71% yield) of sodium allysulfonate. The latter crudeproduct was stirred at zero temperature with 30 mL of POCl3 for 1/2 h then refluxed for 5 h and left to cool toroom temperature. 100 mL of THF was then added to the mixture then filtered off and washed several timeswith dry THF. The filtrate was evaporated carefully on rotavapor and the residue was distilled under vacuum (5mbar). Allylsulfonyl chloride was separated with boiling point range 37-43 oC as coreless oil (71%).

  • 3
  • [ 2495-39-8 ]
  • [ 51116-03-1 ]
YieldReaction ConditionsOperation in experiment
100% With bromine In water at 20℃; for 2h;
With bromine In water
With bromine In water for 2h; Ambient temperature; Yield given;
With bromine In water at 20℃; for 3h; 1.1 1, bromination reaction The mass percentage is 95% sodium allylate 7.5 kg (49 mol) dissolved in 30 kg of pure water.7.8 kg (49 mol) of bromine was added dropwise at room temperature, and the addition was completed in about 2 h. The reaction was stopped at room temperature for 1 h to stop the reaction.A small amount of sodium sulfite was added until the solution became colorless, and the pH was adjusted to 6 to 7 with 20% sodium carbonate to obtain an aqueous solution of sodium 2,3-dibromopropanesulfonate of about 40 L.
With bromine; sodium bromide In water at 20℃; for 3h; Large scale; 1.1 1, bromination reaction 7.5 kg of 95% sodium allyl sulfonate (49 mol) was dissolved in 30 kg of pure water, and 1 kg of sodium bromide (9.72 mol) was added thereto to stir and dissolve at room temperature, and 7.9 kg of bromine (49 mol) was added dropwise, and the addition was completed in about 2 h. The reaction was continued at room temperature for 1 h, the reaction was stopped, a small amount of sodium sulfite was added until the solution became colorless, and the pH was adjusted to 6-7 with 20% sodium carbonate.An aqueous solution of sodium 2,3-dibromopropane sulfonate was obtained in an amount of about 40 L

  • 4
  • [ 106-95-6 ]
  • [ 2495-39-8 ]
YieldReaction ConditionsOperation in experiment
78% With sodium sulfite
76% With sodium sulfite In ethanol; water for 3h; Heating / reflux; 1 Preparation of (Z)-3-(tert-butylamino)prop-1-ene-1-sulfonic acid (Compound N20); To a boiling solution of allyl bromide (21.6 mL, 250 mmol) in a solvent mixture of EtOH and H2O (200 mL, v/v=3:1) was added dropwise a solution of sodium sulfite (15.75 g, 125 mmol) in water (60 mL). The reaction mixture was heated under reflux for 3 hours, and concentrated to dryness under reduced pressure. The obtained white solid was suspended in EtOH in water (130 mL, 90%), heated for 30 minutes, cooled to room temperature, and collected by filtration, giving sodium prop-2-ene-1-sulfonate (14 g, 76%); 1H NMR (500 MHz, D2O) δ 3.55 (d, J=7.3 Hz, 2H), 5.35-5.41 (m, 2H), 5.85-6.00 (m, 1H). To a stirred solution of sulfonate obtained from step 1 (12.0 g, 84 mmol) in water (48 mL) was added bromine (about 4.5 mL) dropwise with stirring until the solution turned pale brown. The solution was stirred at room temperature for 3 hours. A small amount of Na2SO3 was added to destroy the excess bromine. The solvent was then removed in vacuo and a white solid was obtained. Without further purification, the 2,3-dibromo-1-propanesulfonate was treated with concentrated HCl (50 mL) by stirring at room temperature for 1 day. The precipitate (inorganic salt) was removed by filtration. The filtrate was concentrated to yellow syrup. Without further purification, the syrup residue was subjected to vacuum distillation at 140-150° C. to give 2-bromo-1,3-propane sultone (6.5 g, 32%); 1H NMR (500 MHz, CDCl3) δ 3.52 (dd, J=14.0 & 7.0 Hz, 1H), 3.88 (dd, J=14.0 & 7.0 Hz, 1H), 4.50-4.60 (m, 1H), 4.70-4.82 (m, 2H). To a solution of 2-bromo-1,3-propane sultone (obtained in Step 2, 8.0 g, 39.80 mmol) in toluene (200 mL) was added NEt3 (9 mL, 65 mmol). The reaction mixture was stirred for 3 h (or until complete consumption of the starting material), diluted with an aqueous solution of HCl (1 M), and extracted twice with EtOAc. The organic layer was dried over Na2SO4 and concentrated to give 1,3-prop-1-ene sultone (4.5 g, 94%) as a white solid; 1H NMR (500 MHz, CDCl3) δ 5.11 (dd, J=2.2 & 2.2 Hz, 2H), 6.80 (dt, J=6.6 & 2.2 Hz, 1H), 7.00 (dt, J=6.6 & 2.0 Hz, 1H); 13C NMR (125 MHz, CDCl3) δ 72.54, 124.76, 137.04. To a solution of 1,3-prop-1-ene sultone (obtained in step 3, 36 mg, 3 mmol) in THF (5 mL) was added tert-butylamine (316 μL, 3 mmol). The reaction mixture was refluxed for 4 h, and then concentrated to dryness. The residual solid material was suspended in a solvent mixture of EtOH, acetone and ether, heated for 15 minutes, and cooled to room temperature. The solid was collected by filtration, washed with ether then dried, providing the title compound (130 mg, 22%); 1H NMR (500 MHz, D2O) δ 1.24 (s, 9H), 4.00 (d, J=7.0 Hz, 2H), 5.94 (m, 1H), 6.50 (d, J=11.0 Hz, 1H). 13C NMR (125 MHz, D2O) δ 25.08, 37.84, 57.63, 127.81, 136.08. ES-MS 192 (M-1).
75% With sodium sulfite In ethanol; water for 2.5h; Heating;
With sodium sulfite In water for 24h; Reflux;
With sodium sulfite In water at 100℃; 80.1 Step-i: Synthesis of sodium prop-2-ene-i-sulfonate: To a stirred mixture of ally bromide (4.00 g, 33.05 mmol) in water (30 mL), Na2SO3 (8.33 g, 66.11 mmol) was added and heated at 100°C for 6h. The progress of the reaction was monitored by TLC. After completion of the reaction, the reaction mixture was quenched with water and washed with ether. The aqueous layer was concentrated to dryness to afford sodium prop-2-ene-1-sulfonate. Yield: 7 g, crude; NMR: ‘HNMR (400 IVIHz, Deuterium Oxide) 5.97 - 5.95 (m, 1H), 5.29 - 5.06 (m, 2H), 3.17 - 2.89 (m, 2H).
With sodium sulfite In water at 100℃; for 16h; 127.1 Step-1: Synthesis of sodium prop-2-ene-l-sulfonate (190): To a stirred mixture of allyl bromide (15 g, 123.97 mmol) in water (150 mL) was added sodium sulfite (15.7 g, 247.93 mmol) and the reaction mixture was stirred at 100 °C for 16h. Reaction mixture was cooled to room temperature, additional 50 mL of water was added and aqueous layer was extracted with diethyl ether (50 mL x 2). Aqueous layer was concentrated under reduced pressure to afford sodium prop-2-ene-l -sulfonate (22 g crude) as a colourless solid. 1H NMR (400 MHz, D20) δ 3.69 (d, J=7.28 Hz, 2 H), 5.38-5.40 (m, 1 H), 5.44 (d, J=9.03 Hz, 1 H), 5.92 - 6.03 (m, 1 H).
With sodium sulfite In water for 8h; Reflux; Prop-2-ene-1-sulfonyl chloride (1) was prepared by ourmodification on the reported method28 as in the following: To a stirred solution of allyl bromide (12.10 g,0.1mol) in 100 mL distilled water was added Na2SO3 (15 g, 0.12mol). The reaction mixture was refluxed for 8hthen left to cool to room temperature. The reaction mixture was washed with Et2O several times and theaqueous layer was evaporated under reduced pressure. The crude product was washed with methanol,filtered off and left to dry to afford (10.2g, 0.07 mol, 71% yield) of sodium allysulfonate. The latter crudeproduct was stirred at zero temperature with 30 mL of POCl3 for 1/2 h then refluxed for 5 h and left to cool toroom temperature. 100 mL of THF was then added to the mixture then filtered off and washed several timeswith dry THF. The filtrate was evaporated carefully on rotavapor and the residue was distilled under vacuum (5mbar). Allylsulfonyl chloride was separated with boiling point range 37-43 oC as coreless oil (71%).

  • 5
  • [ 2495-39-8 ]
  • [ 769861-83-8 ]
YieldReaction ConditionsOperation in experiment
Stage #1: sodium prop-2-ene-1-sulfonate With bromine In water at 20℃; for 2h; Stage #2: With hydrogenchloride In water at 20℃; for 24h;
  • 6
  • [ 2495-39-8 ]
  • [ 189756-89-6 ]
YieldReaction ConditionsOperation in experiment
32% Stage #1: sodium prop-2-ene-1-sulfonate With bromine In water at 20℃; for 3h; Stage #2: With hydrogenchloride In water at 20℃; for 24h; 1 Preparation of (Z)-3-(tert-butylamino)prop-1-ene-1-sulfonic acid (Compound N20); To a boiling solution of allyl bromide (21.6 mL, 250 mmol) in a solvent mixture of EtOH and H2O (200 mL, v/v=3:1) was added dropwise a solution of sodium sulfite (15.75 g, 125 mmol) in water (60 mL). The reaction mixture was heated under reflux for 3 hours, and concentrated to dryness under reduced pressure. The obtained white solid was suspended in EtOH in water (130 mL, 90%), heated for 30 minutes, cooled to room temperature, and collected by filtration, giving sodium prop-2-ene-1-sulfonate (14 g, 76%); 1H NMR (500 MHz, D2O) δ 3.55 (d, J=7.3 Hz, 2H), 5.35-5.41 (m, 2H), 5.85-6.00 (m, 1H). To a stirred solution of sulfonate obtained from step 1 (12.0 g, 84 mmol) in water (48 mL) was added bromine (about 4.5 mL) dropwise with stirring until the solution turned pale brown. The solution was stirred at room temperature for 3 hours. A small amount of Na2SO3 was added to destroy the excess bromine. The solvent was then removed in vacuo and a white solid was obtained. Without further purification, the 2,3-dibromo-1-propanesulfonate was treated with concentrated HCl (50 mL) by stirring at room temperature for 1 day. The precipitate (inorganic salt) was removed by filtration. The filtrate was concentrated to yellow syrup. Without further purification, the syrup residue was subjected to vacuum distillation at 140-150° C. to give 2-bromo-1,3-propane sultone (6.5 g, 32%); 1H NMR (500 MHz, CDCl3) δ 3.52 (dd, J=14.0 & 7.0 Hz, 1H), 3.88 (dd, J=14.0 & 7.0 Hz, 1H), 4.50-4.60 (m, 1H), 4.70-4.82 (m, 2H). To a solution of 2-bromo-1,3-propane sultone (obtained in Step 2, 8.0 g, 39.80 mmol) in toluene (200 mL) was added NEt3 (9 mL, 65 mmol). The reaction mixture was stirred for 3 h (or until complete consumption of the starting material), diluted with an aqueous solution of HCl (1 M), and extracted twice with EtOAc. The organic layer was dried over Na2SO4 and concentrated to give 1,3-prop-1-ene sultone (4.5 g, 94%) as a white solid; 1H NMR (500 MHz, CDCl3) δ 5.11 (dd, J=2.2 & 2.2 Hz, 2H), 6.80 (dt, J=6.6 & 2.2 Hz, 1H), 7.00 (dt, J=6.6 & 2.0 Hz, 1H); 13C NMR (125 MHz, CDCl3) δ 72.54, 124.76, 137.04. To a solution of 1,3-prop-1-ene sultone (obtained in step 3, 36 mg, 3 mmol) in THF (5 mL) was added tert-butylamine (316 μL, 3 mmol). The reaction mixture was refluxed for 4 h, and then concentrated to dryness. The residual solid material was suspended in a solvent mixture of EtOH, acetone and ether, heated for 15 minutes, and cooled to room temperature. The solid was collected by filtration, washed with ether then dried, providing the title compound (130 mg, 22%); 1H NMR (500 MHz, D2O) δ 1.24 (s, 9H), 4.00 (d, J=7.0 Hz, 2H), 5.94 (m, 1H), 6.50 (d, J=11.0 Hz, 1H). 13C NMR (125 MHz, D2O) δ 25.08, 37.84, 57.63, 127.81, 136.08. ES-MS 192 (M-1).
  • 7
  • [ 2495-39-8 ]
  • nickel(II) sulfide [ No CAS ]
  • [ 7783-06-4 ]
  • [ 7446-09-5 ]
  • [ 7704-34-9 ]
YieldReaction ConditionsOperation in experiment
In water Electrochem. Process; on nickel cathode; pH 2 and 7.5; H2S content depends on pH;
  • 8
  • [ 107-05-1 ]
  • [ 7757-83-7 ]
  • [ 2495-39-8 ]
YieldReaction ConditionsOperation in experiment
In ethanol reflux, 10-12 h;
In ethanol reflux, 10-12 h;
  • 9
  • [ 10025-99-7 ]
  • [ 2495-39-8 ]
  • [ 56-40-6 ]
  • [ 80081-29-4 ]
YieldReaction ConditionsOperation in experiment
With sodium acetate In water-d2 olefin and K2PtCl4 reacted in 1:1 mole ratio in D2O, amino acid and acetate in 1:1 ratio was dissolved in D2O, then evapd. to dryness, to this solid Pt(allylsulfonate)Cl3(2-) dissolved in D2O was added; complexes were monitored by NMR;
  • 10
  • [ 10025-99-7 ]
  • [ 2495-39-8 ]
  • [ 62-57-7 ]
  • [ 80081-34-1 ]
YieldReaction ConditionsOperation in experiment
With sodium acetate In water-d2 olefin and K2PtCl4 reacted in 1:1 mole ratio in D2O, amino acid and acetate in 1:1 ratio was dissolved in D2O, then evapd. to dryness, to this solid Pt(allylsulfonate)Cl3(2-) dissolved in D2O was added; complexes were monitored by NMR;
  • 11
  • [ 10025-99-7 ]
  • [ 56-41-7 ]
  • [ 2495-39-8 ]
  • [ 80081-31-8 ]
YieldReaction ConditionsOperation in experiment
With sodium acetate In water-d2 olefin and K2PtCl4 reacted in 1:1 mole ratio in D2O, amino acid and acetate in 1:1 ratio was dissolved in D2O, then evapd. to dryness, to this solid Pt(allylsulfonate)Cl3(2-) dissolved in D2O was added; complexes were monitored by NMR;
  • 12
  • [ 557-34-6 ]
  • [ 2495-39-8 ]
  • 2,3-dimercapto-propane-1-sulfonic acid ; sodium-zinc-salt [ No CAS ]
YieldReaction ConditionsOperation in experiment
43.2% Stage #1: sodium prop-2-ene-1-sulfonate With bromine; sodium bromide In water at 5℃; for 0.00416667h; Large scale; Stage #2: With sodium hydrogen sulfide; sodium hydroxide In water at 35℃; for 3h; Large scale; Stage #3: zinc diacetate at 78 - 80℃; for 1.5h; Large scale; 4 Example 4 (Preparation of sodium zinc dimercaptopropanesulfonate complex, the amount of adjuvant sodium bromide was increased to 0.3 equivalents) In the present example, the auxiliary sodium bromide was increased from 1.30 kg (12.63 mol, 0.19 equivalents) to 2.05 kg (19.95 mol, 0.30 equivalents), and the other steps and reaction conditions were the same as in Example 1, step a and step b.Results: The consumption of sodium hydroxide 1.20kg (30.01mol), zinc dimercaptopropane sulfonate complex: 5.71kg (20.86mol), liquid purity of 92.7%, 97.1% after deduction of zinc sulfide, calculated as zinc acetate, Yield 45.7%.Example 1 Step a: Preparation of sodium zinc dimercaptopropanesulfonate complexTo 100L glass reactor, add 40.0kg of purified water, open the stirring (medium speed, 100-120rpm),And 0.30 kg (12.63 mol, 0.19 equivalents) of sodium bromide was added to the stirred mixture of 10.36 kg (93%, 66.85 mol, 1.0 equiv.) Of sodium allylsulfonate, and the low temperature cooling circulating pump was opened.Control the internal temperature of 5 ± 3 slowly add 10.0kg bromine (62.58mol, 0.936eq), about 4 hours dripping finished,After the dropwise addition, the mixture was stirred for 10 min. Slowly add 20% sodium hydroxide,Adjust the reaction solution pH to 6-7,A total of 1.30 kg (32.50 mol) of sodium hydroxide was consumed.Add 7.5kg (content 70%, 94.37mol, 1.41 equivalents) sodium hydrosulfide solid, water bath control 35 ± 5 , keep heating for 3 hours, after the end of the insulation, slowly add acetic acid, generate a lot of hydrogen sulfide gas Hydrogen sulfide), adjusted to pH 4-5, and then evacuated for 30 min to remove residual hydrogen sulfide gas from the solution. (0.5.63 mol, 0.68 equivalent) of zinc acetate dihydrate solid was added, stirred and dissolved, heated to 78-80 ° C. After stirring for 1.5 hours, 31.6 kg of ethanol was slowly added to form a large amount of white precipitate. Slow down to 25 , keep warm for 20min, discharge, rejection filter, filter cake at 60 ± 2 blast drying to constant weight, zinc dimercaptopropane sulfonate zinc complex 20.95kg (about 40mol).Step b: Purification of sodium zinc complex of dimercaptopropane sulfonateThe crude product of 10.90 kg of sodium zinc complex of dimercaptopropane sulfonate was dissolved in 21.0 kg of purified water and then transferred to a 100 L glass reactor. The mixture was stirred (medium speed), heated to 79 ± 1 ° C in a water bath and stirred for 20 min, Slowly add 18.0kg of ethanol, and then heated to 79 ± 1 again, after 20min stirring, adjust the water bath temperature, so that the reaction solution temperature slowly dropped to 15 ± 3 , discharge, centrifugal rejection filter to get sodium dimercaptopropanesulfonate Zinc complex is a refined wet product 11.52kg.A solid product of 11.50 kg of sodium dimercaptopropane sulfonate was dissolved in 18.0 kg of purified water and transferred to a 100 L glass autoclave. The mixture was stirred (medium speed), heated to 79 ± 1 ° C in a water bath and Stir the mixture for 20min, slowly add 16.0kg of ethanol, and then heated to 79 ± 1 , 20min after incubation, adjust the temperature of the water bath, the reaction solution temperature slowly dropped to 15 ± 3 , discharge, centrifugal rejection filter to get two mercapto Sodium zinc sulfonate complex secondary purification of wet goods 10.02kg.A mixture of 9.90 kg of dimercaptopropane sulfonate zinc complex was dissolved in 16.0 kg of purified water and then transferred to a 50 L glass reactor. The mixture was stirred (medium speed), heated to 79 ± 1 ° C in a water bath and Heating and stirring for 20min, slowly adding 7.50kg ethanol, and then heated to 79 ± 1 , keep warm for 20min, adjust the temperature of the water bath, the reaction solution temperature slowly dropped to 15 ± 3 , precipitation of white solid, filtration, ethanol washing washing, 60 ± 2 blast drying to constant weight, get dimethoate sodium sulfide zinc complex fine 5.40kg (19.73mol), liquid purity 91.8%, 95.8% after deduction of zinc sulfide, calculated as zinc acetate, the yield of 43.2 %.
  • 13
  • [ 2495-39-8 ]
  • [ 15909-83-8 ]
YieldReaction ConditionsOperation in experiment
With Perbenzoic acid; sulfuric acid; sodium carbonate; citric acid In water at 80℃; for 1h; 1; 2; 3; 4; 5; 6 A method for preparing 1,3-propane sultone, comprising the steps of: (1) Dissolving calcium chloride in deionized water until the solid dissolves, and the mass concentration is15% calcium chloride solution; adding citric acid to the calcium chloride solution, stirring is continued until the solid dissolves, to obtain a mixed solution A;Wherein the mass ratio of the calcium chloride to the citric acid is 5:0.3;(2) Dissolving sodium polyacrylate in deionized water to obtain a mass concentration ofa 3% polyacrylic acid sodium solution, and slowly added it to the mixed solution A prepared above,After the dropwise addition is completed, the mixture is stirred at 3000 rpm for 30 minutes to prepare a mixed solution B; wherein the sodium acrylate solution has a dropping rate of 1 ml/L;The mass ratio of sodium polyacrylate and calcium chloride is 0.1:1;(3) preparing a sodium carbonate solution having a mass concentration of 20%,Then, the mixed solution B prepared above is quickly added to In the sodium carbonate solution, the precipitate was stirred at 5000 rpm.After the end of the precipitation, it was filtered, and the precipitate was washed with deionized water.Drying to obtain porous calcium carbonate;(4) mixing peroxybenzoic acid and deionized water at 50 ° C until the solid dissolves.Then, porous calcium carbonate was added, immersed for 3 hours, and then cooled to room temperature.Drying, preparing a catalyst; wherein, peroxybenzoic acid,The mass ratio of porous calcium carbonate is 1:15;5)Sodium allyl sulfonateMixed with sulfuric acid solutionIn a three-necked flask,Mix and mix for 10 min at a stirring speed of 1500 rpm.Then, the catalyst prepared above was added, and the temperature was slowly raised to 80 ° C.The reaction was stirred for 1 h, and after the reaction was completed, it was cooled to room temperature, and an ethanol solution of sodium hydroxide was added thereto, and the mixture was stirred for 30 minutes, and then acidified with hydrochloric acid.Producing 3-hydroxypropanesulfonic acid; wherein the sodium allylsulfonate,The mass ratio of the catalyst is 10:1; in the ethanol solution of the sodium hydroxide,The mass ratio of sodium hydroxide to ethanol is 5:15
  • 14
  • [ 98-29-3 ]
  • [ 2495-39-8 ]
YieldReaction ConditionsOperation in experiment
98.93% With sodium metabisulfite; N-benzyl-N,N,N-triethylammonium chloride; sodium hydroxide; In water; at 40 - 50℃; under 2250.23 Torr; 930 g of 97% food grade sodium metabisulfite dissolved in 2500 g of deionized water, the temperature of the mixtureRaise to 50 C, stir until sodium metabisulfite is completely dissolved,Add 0.3g of triethylbenzyl chloride to the sodium metabisulfite solutionAmmonium and 0.3 g of polymerization inhibitor p-tert-butyl catechol,After stirring and mixing uniformly, a sodium metabisulfite mixture is obtained;The sodium metabisulfite mixture was passed through three high-precision plungers at a rate of 100 g/min, 1250 g of a 30% sodium hydroxide solution at a rate of 36.44 g/min, and 730 g of allyl chloride at a rate of 21.28 g/min. The metering pump is simultaneously pumped into the microchannel reactor for reaction.Adjust the reaction temperature in the microchannel reactor to 40 C,Adjusting the back pressure valve to make the pressure of the microchannel reactor0.3 MPa, the reaction-reacted crude product was filtered through a fine filter, and 538 g of a clear liquid was collected.The sample was analyzed by HPLC analysis, and the content of sodium allylsulfonate in the product obtained by the method of the present example was25.03%, the yield is 98.93% based on chloropropene.The Hull cell test piece passed the test.
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Similarity: 0.81

Chemical Structure| 2695-37-6

[ 2695-37-6 ]

Sodium 4-vinylbenzenesulfonate

Similarity: 0.52

Chemical Structure| 304675-74-9

[ 304675-74-9 ]

Sodium 4-vinylbenzenesulfonate hydrate

Similarity: 0.52

Chemical Structure| 52556-42-0

[ 52556-42-0 ]

Sodium 3-(allyloxy)-2-hydroxypropane-1-sulfonate

Similarity: 0.50

Aliphatic Chain Hydrocarbons

Chemical Structure| 1561-92-8

[ 1561-92-8 ]

Sodium 2-methylprop-2-ene-1-sulfonate

Similarity: 0.81

Chemical Structure| 5325-43-9

[ 5325-43-9 ]

Sodium ethane-1,2-disulfonate

Similarity: 0.72

Chemical Structure| 2386-53-0

[ 2386-53-0 ]

Sodium dodecane-1-sulfonate

Similarity: 0.71

Chemical Structure| 22767-49-3

[ 22767-49-3 ]

Sodium pentane-1-sulfonate

Similarity: 0.71

Chemical Structure| 2386-54-1

[ 2386-54-1 ]

Sodium butane-1-sulfonate

Similarity: 0.71