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CAS No. : | 41840-28-2 | MDL No. : | MFCD00006080 |
Formula : | C11H16N2O2S | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | POTDIELOEHTPJN-UHFFFAOYSA-N |
M.W : | 240.32 | Pubchem ID : | 148428 |
Synonyms : |
|
Num. heavy atoms : | 16 |
Num. arom. heavy atoms : | 6 |
Fraction Csp3 : | 0.55 |
Num. rotatable bonds : | 4 |
Num. H-bond acceptors : | 4.0 |
Num. H-bond donors : | 0.0 |
Molar Refractivity : | 64.62 |
TPSA : | 77.38 Ų |
GI absorption : | High |
BBB permeant : | Yes |
P-gp substrate : | No |
CYP1A2 inhibitor : | Yes |
CYP2C19 inhibitor : | Yes |
CYP2C9 inhibitor : | No |
CYP2D6 inhibitor : | No |
CYP3A4 inhibitor : | No |
Log Kp (skin permeation) : | -5.62 cm/s |
Log Po/w (iLOGP) : | 3.07 |
Log Po/w (XLOGP3) : | 3.02 |
Log Po/w (WLOGP) : | 3.12 |
Log Po/w (MLOGP) : | 1.13 |
Log Po/w (SILICOS-IT) : | 2.49 |
Consensus Log Po/w : | 2.56 |
Lipinski : | 0.0 |
Ghose : | None |
Veber : | 0.0 |
Egan : | 0.0 |
Muegge : | 0.0 |
Bioavailability Score : | 0.55 |
Log S (ESOL) : | -3.25 |
Solubility : | 0.136 mg/ml ; 0.000567 mol/l |
Class : | Soluble |
Log S (Ali) : | -4.31 |
Solubility : | 0.0118 mg/ml ; 0.000049 mol/l |
Class : | Moderately soluble |
Log S (SILICOS-IT) : | -3.44 |
Solubility : | 0.0865 mg/ml ; 0.00036 mol/l |
Class : | Soluble |
PAINS : | 0.0 alert |
Brenk : | 1.0 alert |
Leadlikeness : | 1.0 |
Synthetic accessibility : | 2.76 |
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-H335 | Packing Group: | N/A |
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 |
---|---|---|
85.5% | With hydrogenchloride In chloroform | 1) Synthesis of N-t-butoxycarbonylallylamine (27) Allylamine [2.855 g (50 mmol.)] was dissolved in chloroform (100 m), to which was added t-butyl S-(4,6-dimethylpyrimidin-2-yl)thiocarbonate [12.017 g (50 mmol.)], and then the mixture was stirred at room temperature for 24 hours. 1N Hydrochloric acid was added to the reaction mixture, which was subjected to extraction with chloroform. The organic layer was dried over anhydrous potassium carbonate, and then concentrated under reduced pressure. The crude product thus obtained was purified by column chromatography (silica gel: 240 g; eluent: hexane.ethyl acetate = 3/1) to obtain the desired product (27) [6.720 g (85.5percent, colorless prisms, m.p. 34 to 34.8°C)]. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
93% | With triethylamine In 1,4-dioxane; water for 6h; Ambient temperature; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
89.9% | With triethylamine In water; N,N-dimethyl-formamide |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
88% | In water; N,N-dimethyl-formamide for 8h; Ambient temperature; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
76% | With triethylamine In 1,4-dioxane; water Ambient temperature; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
74% | In tetrahydrofuran at 70℃; for 1h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
81.3% | With triethylamine In 1,4-dioxane; water at 20℃; for 6h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
89% | With triethylamine In water Ambient temperature; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With triethylamine In 1,4-dioxane; water | ||
With triethylamine In 1,4-dioxane; water for 16h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
87% | With triethylamine In 1,4-dioxane; water for 23h; Ambient temperature; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With triethylamine In 1,4-dioxane; water for 24h; Ambient temperature; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
95% | With triethylamine In 1,4-dioxane; water for 24h; Ambient temperature; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With triethylamine In 1,4-dioxane; water Yield given; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
90% | With triethylamine In 1,4-dioxane; water for 6h; Ambient temperature; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
92% | With triethylamine In 1,4-dioxane; water for 6h; Ambient temperature; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
92% | With triethylamine In 1,4-dioxane; water for 6h; Ambient temperature; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
87% | With triethylamine In 1,4-dioxane; water for 16h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
67% | With triethylamine In 1,4-dioxane; water at 20℃; for 12h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
77% | In dichloromethane |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
95.4% | With triethylamine In 1,4-dioxane; water for 15h; Ambient temperature; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
90% | With triethylamine In 1,4-dioxane; water for 6h; Ambient temperature; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
96% | With triethylamine In 1,4-dioxane; water for 6h; Ambient temperature; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
95% | With triethylamine In 1,4-dioxane; water for 6h; Ambient temperature; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
80% | In tetrahydrofuran for 24h; Ambient temperature; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With triethylamine In tetrahydrofuran at 25℃; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
94% | With triethylamine In 1,4-dioxane; water for 6h; Ambient temperature; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
96.6% | With triethylamine In 1,4-dioxane; water for 12h; Ambient temperature; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
90% | With triethylamine In 1,4-dioxane; water for 6h; Ambient temperature; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
89% | With triethylamine In 1,4-dioxane; water | |
With iodine; sodium hydrogencarbonate; triethylamine; potassium iodide 1.) dioxane, water, 2.) water; Multistep reaction; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With triethylamine In 1,4-dioxane; water at 25℃; Yield given; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
64% | With triethylamine In tetrahydrofuran; water for 24h; Ambient temperature; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
95% | In dichloromethane for 48h; Ambient temperature; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
95% | In 1,4-dioxane at 20℃; for 9h; | 2.11. Synthesis of [3-[3-(Aminopropyl)methylamino]propyl]carbamic acid tert-butyl ester (9) 9 was synthesized according to the previous report [10], N,N′ -bis(3-aminopropyl)methylamine (24.8 mL, 166 mmol) was dissolved indioxane (200 mL) and S-Boc-2-mercapto-4,6-dimethylpyrimidine (10 g,42 mmol) in dioxane (160 mL) was added dropwise to this solution. Theprecipitate that formed during the dropwise addition was taken up in asmall amount of water. After stirring for 9 h, the water was evaporatedunder reduced pressure. A saturated saline solution (140 mL) was addedto the residue, followed by extraction with ethyl acetate (50 mL). Theorganic phase was dried over anhydrous MgSO4 and evaporated underreduced pressure to give 9 as a yellow viscous oil (9.7 g, 40 mmol, 95%yield). 1H NMR (500 MHz, CDCl3): δ = 1.44 (9H, s, t-Bu), 1.60-1.65 (4H,m, CH2CH2CH2N(CH3)CH2CH2CH2), 2.19 (3H, s, CH2N(CH3)CH2),2.37-2.40 (4H, m, CH2N(CH3)CH2), 2.74 (2H, t, J = 5.9 Hz, H2NCH2),3.18 (2H, q, J = 5.9 Hz, CH2NHCO), and 5.42 (1H, br, NHCO) ppm (Fig.S16). HRMS (EI+) m/z [M]+ Calcd for C12H28N3O2 246.21815, found246.21785. |
32% | In 1,4-dioxane at 20℃; for 20h; | |
25% | In 1,4-dioxane |
In 1,4-dioxane |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With triethylamine In 1,4-dioxane; water at 20℃; for 26h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With triethylamine In 1,4-dioxane; water at 20℃; for 26h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 4 steps 1: 89 percent / Et3N / H2O / Ambient temperature 2: 95 percent / dicyclohexylamine / dimethylformamide; CH2Cl2 / Ambient temperature 3: 77 percent / p-toluensulfonic acid monohydrate / CH2Cl2 / 4 h / Ambient temperature 4: 100 percent / H2 / 10percent Pd/C / ethanol / Ambient temperature |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 6 steps 1: 89 percent / Et3N / H2O / Ambient temperature 2: 95 percent / dicyclohexylamine / dimethylformamide; CH2Cl2 / Ambient temperature 3: 77 percent / p-toluensulfonic acid monohydrate / CH2Cl2 / 4 h / Ambient temperature 4: 100 percent / H2 / 10percent Pd/C / ethanol / Ambient temperature 5: 1.) N,N-dicarbonyldiimidazole (DCI) / 1.) THF, RT, 6 h, 2.) THF, RT, overnight 6: 1.) tert-BuOK, EtBr, 2.) H2 / 2.) 10percent Pd/C / 1.) tert-BuOH, 50 deg C, overnight, 2.) EtOH, RT, overnight |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 5 steps 1: 89 percent / Et3N / H2O / Ambient temperature 2: 95 percent / dicyclohexylamine / dimethylformamide; CH2Cl2 / Ambient temperature 3: 77 percent / p-toluensulfonic acid monohydrate / CH2Cl2 / 4 h / Ambient temperature 4: 100 percent / H2 / 10percent Pd/C / ethanol / Ambient temperature 5: 1.) N,N-dicarbonyldiimidazole (DCI) / 1.) THF, RT, 6 h, 2.) THF, RT, overnight |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 2: dicyclohexylcarbodiimide; 1-hydroxytriazole; / CH2Cl2 |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 2: 54 percent / dicyclohexylcarbodiimide; 1-hydroxybenzotriazole; / CH2Cl2 / 1) 3 h; 0 deg C; 2) 15 h; room temp. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 2: triethylamine; 1-hydroxybenztriazole; dicyclohexylcarbodiimide; / CH2Cl2 |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 2: triethylamine; 1-hydroxybenztriazole; dicyclohexylcarbodiimide; / CH2Cl2 / 1) 3 h; 0 deg C; 2) 15 h; room temp. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 2: triethylamine; 1-hydroxybenztriazole; dicyclohexylcarbodiimide; / CH2Cl2 |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 1: 81.3 percent / Et3N / dioxane; H2O / 6 h / 20 °C 2: 67.9 percent / NH3 / ethanol | ||
Multi-step reaction with 2 steps 1: 81.3 percent / Et3N / dioxane; H2O / 6 h / Ambient temperature 2: 67.9 percent / NH3 / ethanol / Heating |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 1: Et3N / dimethylformamide; H2O / 20 h / Ambient temperature 2: 1) N-hydroxysuccinimide, DCC, 2) aq. NH3 / 1) CH3CN, room temperature, 2 h, 2) 4 deg C, 30 min |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 3 steps 1: 7.00 g / Et3N / H2O; dimethylformamide 2: 86.8 percent / dicyclohexylcarbodiimide (DCC) / ethyl acetate / 2 h / 0 °C 3: 70.8 percent / 25percent aq. ammonia / tetrahydrofuran / 2 h / Ambient temperature |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 1: 7.00 g / Et3N / H2O; dimethylformamide 2: 86.8 percent / dicyclohexylcarbodiimide (DCC) / ethyl acetate / 2 h / 0 °C |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 1: dioxane 2: Et3N / methanol |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 1: dioxane 2: Et3N / CHCl3 |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
99.9% | In chloroform | P.13.1 1) 1) Synthesis of N-t-butoxycarbonyl-2-(2--hydroxyethyl) piperidine (33) 2-(Piperidin-2-yl)ethanol [3.23 g (25 mmol.)] was dissolved in chloroform (50 ml), to which was added t-butyl S-(4,6-dimethylpyrimidin-2-yl)thiocarbonate [6.01 g (25 mmol.)], and the mixture was stirred at room temperature for 40 hours. The reaction mixture was refluxed for further 4 hours. The reaction mixture was cooled, and subjected to extraction with chloroform after 1N hydrochloric acid was added. The organic layer was dried over anhydrous potassium carbonate, which was then concentrated under reduced pressure. The crude product thus obtained was purified by column chromatography (silica gel: 200 g; solvent: hexane/ethyl acetate = 2/1) to obtain the desired product (33) [5.73 g (99.9%, pale yellow oily substance)]. |
In chloroform | P.13.1 (1) (1) Synthesis of N-t-butoxycarbonyl-2-(2'-hydroxyethyl)piperidine (33) 2-(Piperidin-2-yl)ethanol[3.23 g(25 mmol.)] was dissolved in chloroform(50 ml), to which was added t-butyl S-(4,6-dimethylpyrimidin-2-yl)thiocarbonate[6.01 g(25 mmol.)], and the mixture was stirred at room temperature for 40 hours. The reaction mixture was refluxed for further 4 hours. The reaction mixture was cooled, and subjected to extraction with chloroform after 1N hydrochloric acid was added. The organic layer was dried over anhydrous potassium carbonate, which was then concentrated under reduced pressure. The crude product thus obtained was purified by column chromatography (silica gel:200 g;solvent:hexane/ethyl acetate=2/1) to obtain the desired product(33)[5.73 g(99.9%, pale yellow oily substance)]. TLC[Silica Gel:hexane/AcOEt(2/1)]:Rf=0.24. NMR(90 MHz,CDCl3) δ: 1.45(9H,s,CH3 x3), 1.58(6H,m,CH2 x3), 1.92 (2H,m,CH2 CH2 OH), 2.68(1H,m,CHNBOC), 3.52(2H,m,CH2 OH), 3.95(1H,m,CHNBOC), 4.45(1H,m,CHNBOC). IR(film)cm-1: 3440, 2940, 2860, 1690, 1660, 1420, 1363, 1275, 1162, 1140, 1052. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In chloroform | P.1.1 (1) (1) Synthesis of N-(3-t-butoxycarbonylaminopropyl)diethanolamine(1) N-(3-Aminopropyl)diethanolamine[4.725 g(29.127 mmol.)] was dissolved in chloroform(50 ml), to which was added a solution of t-butyl S-(4,6-dimethylpyrimidin-2-yl)thiocarbonate [7.00 g (29.127 mmol.)] in chloroform(50 ml), and then the mixture was stirred at room temperature for 19 hours. The reaction mixture was concentrated under reduced pressure, and the crude product thus obtained was purified by column chromatography(silica gel: 300 g; eluent:chloroform/methanol=5/1→1/1) to obtain the desired product(1)[6.776 g(88.5%)] (pale yellow oily compound). TLC(Silica Gel; CHCl3 /MeOH(1/1): Rf=0.34. NMR(90 MHz,CDCl)δ: 1.42(9H,s), 1.63(2H, quint), 2.60(6H,m), 3.19(4H,t), 3.87(2H,s), 5.30(1H,br). IR(film)cm-1: 3330, 2950, 2860, 2810, 1690, 1525, 1365, 1280, 1255, 1170, 1040, 758. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With potassium hydroxide In chloroform | P.2.i (i) (i) Synthesis of N-tert-butoxycarbonyl-N-phenylaminoethanol(6) In chloroform(40 ml) was dissolved β-anilinoethanol[6.32 ml(50 mmol.)]. To the solution was added tert-butyl S-(4,6-dimethylpyrimidin-2-yl)thiocarbonate[13.10 g(60 mmol.)]. and the mixture was heated for two hours under reflux. The reaction mixture was cooled and washed with a 5% aqueous solution of potassium hydroxide. The organic layer was dried over anhydrous potassium carbonate, then the solvent was distilled off under reduced pressure. The crude product thus obtained was purified by means of a column chromatography (silica gel:180 g; eluent:n-hexane/ethyl acetate=2/1) to afford the object compound(6)[11.257 g(94.9%, colorless solid matter)]. TLC(Silica Gel;n-hexane/AcOEt=1/1) Rf=0.53. NMR(90 MHz,CDCl3) δ: 1.42(9H,s),2.79(1H,br),(3.78(4H,m), 7.26(5H,m). IR(KBr)cm-1: 3460,1668,1590,1395,1165. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
85.5% | With hydrogenchloride In chloroform | P.11.1 1) 1) Synthesis of N-t-butoxycarbonylallylamine (27) Allylamine [2.855 g (50 mmol.)] was dissolved in chloroform (100 ml), to which was added t-butyl S-(4,6-dimethylpyrimidin-2-yl)thiocarbonate [12.017 g (50 mmol.)], and then the mixture was stirred at room temperature for 24 hours. 1N Hydrochloric acid was added to the reaction mixture, which was subjected to extraction with chloroform. The organic layer was dried over anhydrous potassium carbonate, and then concentrated under reduced pressure. The crude product thus obtained was purified by column chromatography (silica gel: 240 g; eluent: hexane.ethyl acetate = 3/1) to obtain the desired product (27) [6.720 g (85.5%, colorless prisms, m.p. 34 to 34.8°C)]. |
With hydrogenchloride In chloroform | P.11.1 (1) (1) Synthesis of N-t-butoxycarbonylallylamine(27) Allylamine[2.855 g(50 mmol.)]was dissolved in chloroform (100 ml), to which was added t-butyl S-(4,6-dimethylpyrimidin-2-yl)thiocarbonate[12.017 g(50 mmol.)], and then the mixture was stirred at room temperature for 24 hours. 1N Hydrochloric acid was added to the reaction mixture, which was subjected to extraction with chloroform. The organic layer was dried over anhydrous potassium carbonate, and then concentrated under reduced pressure. The crude product thus obtained was purified by column chromatography(silica gel: 240 g;eluent:hexane.ethyl acetate=3/1) to obtain the desired product(27)[6.720 g(85.5%,colorless prisms, m.p.34 to 34.8° C.)]. TLC[Silica Gel;hexane/AcOEt(4/1)]:Rf=0.22. NMR(90 MHz,CDCl3) δ: 1.45(9H,s,CH3 x3), 3.72(2H,m,CH2), 4.79 (1H,br.NH), 5.15(2H,m,=CH2), 5.65 to 6.07[1H,m,CH=). IR(KBr)cm-1: 3320, 2960, 2900, 1670, 1510, 1360, 1245, 1150, 1040, 1015, 990, 950, 922, 860. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In chloroform; ethyl acetate; | (1) Synthesis of N-(t-butoxycarbonyl)diethanolamine(17) Diethanolamine[10.51 g(0.1 mol.)]was dissolved in chloroform(200 ml), to which was added t-butyl S-(4,6-dimethyl pyrimidin-2-yl)thiocarbonate[24.03 g(0.1 mol.)], and the mixture was stirred at room temperature for 24 hours. The reaction mixture was concentrated under reduced pressure. Ethyl acetate was added to the residue, and the resulting precipitates were filtered off, then the filtrate was concentrated under reduced pressure. The crude product thus obtained was purified by column chromatography(silica gel: 500 g;eluent:ethyl acetate/acetone=6/1?5/1) to obtain the desired product(17)[17.85 g(87.0%, pale yellow oily substance)] TLC(Silica Gel;AcOEt/acetone(5/1):Rf=0.33. NMR(90 MHz,CDCl3) delta: 1.45(9H,s,CH3 x3), 3.40(4H,t,CH2 Nx2), 3.76(4H,m,CHzOx2), 4.38(2H,br.s,OHx2). IR(film)cm-1: 3350(br), 2975, 2925, 2870, 1670, 1480, 1415, 1369, 1258, 1230, 1163, 1140, 1050. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
77.9% | In chloroform; ethyl acetate | P.1.i (i) (i) Synthesis of N-methyl-N-tert-butoxycarbonylaminoethanol(1) In chloroform(50 ml) was dissolved N-methylethanolamine [2.81 ml(35 mmol.). To the solution was added tert-butyl S-(4,6-dimethylpyrimidin-2-yl)thiocarbonate[8.42 g(35 mmol.)], and the mixture was stirred at room temperature for 24 hours. The reaction mixture was concentrated under reduced pressure. To the concentrate was added ethyl acetate, and insolubles were filtered off, and the filtrate was concentrated under reduced pressure. The crude product thus obtained was purified by means of a column chromatography(silica gel:140 g; eluent:n-hexane/ethyl acetate=1/2) to obtain the object compound (1)[4.78 g(77.9%; yellow oily substance)]. TLC(Silica Gel: n-hexane/AcOEt=1/5)Rf=0.40. NMR(90 MHz, CDCl3) δ: 1.44(9H,s), 2.89(3H,s), 3.29(2H,t), 3.64(2H,t). IR(Neat)cm-1: 3400,2970,2925,1670,1480,1390,1362,1150. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In 1,4-dioxane; chloroform; ethyl acetate | 15.1 EXAMPLE 15 (1) 1.01 g of 2-tert.-butoxycarbonylthio-4,6-dimethylpyrimidine are added under ice-cooling to a solution of 1.59 g of (-)-cis-2-(4-methoxyphenyl)-3-hydroxy-5-[2-(N-methylamino)-ethyl]-8-chloro-2,3-dihydro-1,5-benzothiazepin-4(5H)-one in 10 ml of dioxane, and the mixture is stirred at room temperature for 2 hours. Then, the mixture is diluted with water, and the aqueous mixture is extracted with a mixture of chloroform and ethyl acetate (1:1). The extract is washed with 10% hydrochloric acid and water, dried and then evaporated to remove solvent. The residue is purified by silica gel chromatography, whereby 1.05 g of (-)-cis-2-(4-methoxyphenyl)-3-hydroxy-5-[2-(N-tert.-butoxycarbonyl-N-methylamino)ethyl]-8-chloro-2,3-dihydro-1,5-benzothiazepin-4(5H)-one are obtained as an oil. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
93% | With triethylamine In tetrahydrofuran; water | 39.1 (1) (1) 4-(N-t-Butoxycarbonyl-N-methylaminomethyl)2,3,4,9-tetrahydrothiopyrano[2,3-b]indole To a solution of 4-methylaminomethyl-2,3,4,9-tetrahydrothiopyrano[2,3-b]indole (4.41 g) in tetrahydrofuran (50 ml) are added triethylamine (4 ml) and 2-(t-butoxycarbonylthio)-4,6-dimethylpyrimidine (4.76 l g) successively at room temperature. The mixture is stirred at room temperature for 2.5 hours and evaporated to remove the solvent. The residue is extracted with chloroform after addition of water. The extract is washed, dried and evaporated to give crude crystals. Recrystallization from acetone gives the title compound (5.57 g) melting at 220°-222° C. (decomp.). Yield: 93%. IR: νmaxCHCl3 3460, 1675 cm-1. Anal. Calcd. for C18 H24 N2 O4 S: C, 65.03; H, 7.28; N, 8.43; S, 9.64. Found: C, 64.94; H, 7.28; N, 8.32; S, 9.65. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
685 mg (68.7%) | With triethanolamine; In diethyl ether; ethanol; water; acetonitrile; | EXAMPLE 26 Production of Boc-Tyr-Gly-Gly-Phe-Met-OH In 5 ml of 50% aqueous acetonitrile were dissolved 900 mg of <strong>[58569-55-4]H-Tyr-Gly-Gly-Phe-Met-OH</strong>. To the solution was added 0.52 ml of TEA. The mixture was cooled with ice, to which were added 720 mg of Boc-SDP, followed by stirring for 15 hours. The solvent was distilled off. The residue was dissolved in 10 ml of water, and the solution was washed with AcOEt. The aqueous layer was concentrated. To the residue were added 2 ml each of acetic acid and 80% EtOH. The mixtue was placed on a column (3*48 cm) of Sephadex LH-20. Elution was conducted with 80% EtOH, and fractions of 200 to 235 ml were collected and concentrated. The concentrate was dissolved in 30 ml of water and the solution was acidified with AcOH, which was then subjected to extraction with AcOEt. The extract was washed with water and dried over anhydrous sodium sulfate. The solvent was distilled off, and to the residue was added diethyl ether. The resulting powdery product was recovered by filtration and recrystallized from AcOEt. Yield 685 mg (68.7%); m.p. 159-160 C. (decomp.); [alpha]D24 -16.8 (c=0.94, DMF); Rf1 =0.21, Rf2 =0.68, Rf3 =0.41. Elemental analysis, for C32 H43 O9 N5 S: Calcd.: C, 57.04; H, 6.43; N, 10.40; S, 4.76; Found: C, 56.58; H, 6.47; N, 10.25; S, 4.76 |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
85% | In tetrahydrofuran; methanol; dichloromethane | 22 EXAMPLE 22 EXAMPLE 22 A mixture of 1 g of 1-[3-(4-amino-2-methoxyphenoxy)-n-propyl]-4-phenyl-piperazine, 1.06 g of 2-(t-butoxycarbonylthio)-4,6-dimethylpyrimidine and 15 ml of anhydrous tetrahydrofuran is refluxed for 65 hours. After the reaction, the mixture is evaporated under reduced pressure to remove tetrahydrofuran. Methylene chloride is added to the residue, and the mixture is washed with an aqueous 10% sodium hydroxide solution and water, successively. Said mixture is dried and then evaporated under reduced pressure to remove the solvent. The residue is purified by silica gel chromatography (Solvent; 1.5% methanol/chloroform), and then recrystallized from a mixture of benzene and n-hexane. 1.31 g of 1-[3-(4-t-butoxycarbonylamino-2-methoxyphenoxy)-n-propyl]-4-phenyl-piperazine are thereby obtained as colorless needles. Yield: 85% M.p. 125° C.-126.5° C. IRνmaxNujol (cm-1): 3350, 1690, 1160, 1000 NMR (CDCl3)δ: 7.44-6.6 (m, 9H, aromatic and --NH--), 4.09 (t, 2H, J=6.5 Hz, --OCH2 CH2 --), 3.87 (s, 3H, --OCH3), 3.4-3.1 (m, 4H), 2.7-1.5 (m, 6H), 1.51 (s, 9H, --C(CH3)3) Mass m/e: 441 (M+), 175 (base peak) |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In pyridine; methanol; chloroform; water | b EXAMPLE (b) Synthesis of O-tosyl-3-tert-butoxycarbonylamino-1-propanol. Into 30 mL of methanol, was dissolved 1.5 g (20 mmoles) of 3-amino-1-propanol followed by the addition of 4.8 g (20 mmoles) of tert-butyl S-4,6-dimethylpyrimid-2-yl thiocarbonate (a product of Kokusan Kagaku Co.). The mixture was stirred for 6 hours. The reaction mixture was evaporated to dryness, dissolved in 200 mL of chloroform, and washed with 200 mL of water. The chloroform layer was concentrated and subjected to column chromatography using 300 g of silica gel (Wako-GelC-200) and a toluene-ethyl acetate (1:1 by volume) mixture as developing solvent. Fraction Nos. 82 to 151 (each 15 mL in volume) were combined, evaporated to dryness to obtain 2.95 g (84% yield) of 3-tert-butoxycarbonylamino-1-propanol in colorless oily form. Into 50 mL of pyridine was dissolved 2.95 g (16.9 mmoles) of 3-tert-butoxycarbonylamino-1-propanol. To the solution, while being cooled in ice under an argon atmosphere, was added dropwise over a period of 40 minutes a solution of 3.36 g (17.7 mmoles) of p-toluenesulfonyl chloride in pyridine. The mixture was left standing overnight at 7° C., then admixed with a small volume of water, and evaporated to dryness. The residue was dissolved in 200 mL of chloroform, washed successively with 5% aqueous potassium hydrogensulfate solution, saturated aqueous sodium hydrogencarbonate solution, and water, then dried over anhydrous sodium sulfate, evaporated to dryness, and subjected to column chromatography using 120 g of silica gel (Wako-GelC-200) and a toluene-ethyl acetate (8:1 by volume) mixture as developing solvent. Fraction Nos. 35 to 68 (each 15 mL in volume) were combined and evaporated to dryness to yield 3.06 g (55% yield) of O-tosyl-3-tert-butoxycarbonylamino-1-propanol in colorless oily form. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With ammonium hydroxide In 1,4-dioxane; water | C 1-(3-Aminopropyl)-4-(-tert-butoxycarbonylaminopropyl)piperazine III 1-(3-Aminopropyl)-4-(-tert-butoxycarbonylaminopropyl)piperazine III A solution of 100 g (0.42 mol) of tert-butyl S-(4,6-dimethylpyrimidin-2-yl) thiolcarbonate (II) available from Aldrich Chemical, in 400 ml of dry dioxane was added at room temperature, dropwise over a period of 6 hours, to a solution of 182 g (0.91 mol) of 1,4-bis-(3-aminopropyl) piperazine (I) in 360 ml of dioxane. After stirring overnight, the reaction was filtered and evaporated to give a yellow oil. It was dissolved in 2 liters of distilled water and applied to a 90 cm*5 cm column of Amberlite IRC-50 ion exchange resin (NH4≈ form). The column was washed with 500 ml of water, then eluted with a linear gradient of 2 liters of water to 2 liters of 0.5 M ammonium hydroxide. The appropriate fractions were pooled and evaporated to give 65 g of the amine (III) as a light-yellow oil. Analysis: Mass Spectrum (70 e.V.): m/e 301 [MH+ ]; 201 [MH+ minus COOC(CH3)3 ]. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With hydrogenchloride; sodium hydrogencarbonate; triethylamine; citric acid In 1,4-dioxane; water; ethyl acetate | 39 8-tert-Butyloxycarbonyl-2-hydroxy-2,8-diazaspiro[4,5]decane-1,3-dione EXAMPLE 39 8-tert-Butyloxycarbonyl-2-hydroxy-2,8-diazaspiro[4,5]decane-1,3-dione In a mixture solvent consisting of water (50 ml) and dioxane (50 ml) was dissolved 2-hydroxy-2,8-diazaspiro[4,5]decane-1,3-dione.hydrochloride (8.35 g). To the solution were added triethylamine (14 ml) and 2-(tert. butyloxycarbonylthio)-4,6-dimethylpyrimidine (9.6 g). The mixture was stirred for 2 hours at room temperature. The solvent was evaporated off under reduced pressure, and the residual oil was evaporated in 100 ml of ethyl acetate. To the solution was added 100 ml of a saturated aqueous solution of sodium hydrogencarbonate. The aqueous layer was made acid with a solid citric acid, followed by extraction with 100 ml of ethyl acetate. The organic layer was washed with 50 ml of 1N hydrochloric acid and water, which was then dried over anhydrous magnesium sulfate, followed by evaporating off the solvent to leave an oil. This oil was solidified with diethyl ether-n-hexane, which was collected by filtration to obtain 9.6 g of a colorless solid, m.p. 151° to 154° C. Elemental analysis (as C13 H20 N2 O5): Calculated: C, 54.92; H, 7.09; N, 9.85 Found: C, 54.90; H, 7.17; N, 9.67. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With sodium chloride In 1,4-dioxane; water | 1.a (a) (a) Synthesis of N-(6-aminohexyl)maleimide hydrochloride In 90 ml of dioxane was dissolved 23.20 g (0.20 mole) of 1,6-diaminohexane and a solution of 24.60 g 0.10 mole) of 2-(t-butoxycarbonylthio)-4,6-dimethylpyrimidine in 100 ml of dioxane was added dropwise thereto over a period of 3 hours. After completion of dropwise addition, the mixture was stirred overnight. The reaction mixture was filtered to separate the precipitate and the filtrate was concentrated to about 100 ml. This concentrate was diluted with 150 ml of water and the precipitated bis(N,N--t-butoxycarbonyl)-1,6-diaminohexane was filtered off. The resulting filtrate was concentrated under reduced pressure to about half the initial volume. To the concentrate was added 40 g of sodium chloride and the mixture was extracted 4 times with 50 ml of ethyl acetate. The extracts were pooled and the ethyl acetate was distilled off under reduced pressure. The residue was dissolved in 100 ml of water and the solution was adjusted to pH about 3 with 1N-hydrochloric acid. This aqueous solution was washed with ethyl acetate a few times and sodium chloride was added to the aqueous layer to precipitate N-t-butoxycarbonyl-1,6-diaminohexane hydrochloride. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
88% | In 1,4-dioxane for 18h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
63% | In tetrahydrofuran for 33h; Reflux; Inert atmosphere; | 4.4. N-Boc protection of 6: synthesis of 7 (Scheme 4) Anhydrous THF (0.2 mL, 0.8 M) and S-Boc-2-mercapto-4,6-dimethylpyrimidine (Boc-S) (42 mg, 0.173 mmol, 1.3 equiv) were added to 6 (54.4 mg, 0.133 mmol), which had been dried under vacuum for 5 min. The mixture was refluxed for 21 h, then an additional amount of Boc-S (16 mg, 0.066 mmol, 0.5 equiv) and THF (0.2 mL) were added the reaction mixture was refluxed for another 12 h. Removal of the solvent left a residue, which was dissolved in EtOAc and then washed with 3 mL of a 1% aqueous solution of citric acid (pH ∼2-3). The organic layer was washed with 5% aqueous solution of NaHCO3 (3 mL, pH=8) and brine (pH=7) and finally dried over Na2SO4. After filtration and concentration, the residue was purified through silicagel (petroleum ether/EtOAc 10:1 then 6:1) to give 7 as an oil (43.1 mg, 0.084 mmol) in 63% yield. Rf=0.60 (Petroleum ether/EtOAc=6:1-Ceric Ammonium Molybdate); -58.1 (c 2 in chloroform); 1H NMR (300 MHz, acetone-d6, TMS): δ=7.28 (d, 3J(H,H)=7.8 Hz, 0.6H, rotamer of 2, 4), 7.22 (d, 3J(H,H)=7.8 Hz, 2H, 2, 4), 6.90 (d, 3J(H,H)=7.8 Hz, 0.3H, rotamer of 3), 6.84 (dd, 3J(H,H)=7.8 and 7.5 Hz, 1H, 3), 5.24 (s, 1H, 8), 5.11 (s, 0.3H, rotamers of 8), 4.19 (q, 3J(H,H)=6.9 Hz, 2H, 13, overlapped with its rotamer), 4.01 (dd, 3J(H,H)=7.5 and 7.2 Hz, 1H, 11), 3.44 (s, 3H, 7), 3.38 (s, 0.9H, rotamer of 7), 2.62 (dd, 3J(H,H)=12.9 and 7.5 Hz, 1H, part of AB system, 10a), 2.41 (dd, 3J(H,H)=12.9, 7.2 Hz, 1H, part of AB system, 10b), 1.54 (s, 2.7H, rotamer of 18), 1.42 (s, 9H, 18), 1.29 (t, 3J(H,H)=7.2 Hz, 3H, 14), 1.24 (t, 3J(H,H)=6.9 Hz, 0.9H, rotamer of 14), 0.88 (t, 3J(H,H)=7.8 Hz, 11.7H, 16 overlapped with its rotamer), 0.50 (q, 3J(H,H)=7.8 Hz, 7.8H, 15 overlapped with its rotamer); 13C NMR (75 MHz, acetone-d6, TMS): δ=173.4 (12), 172.5 (rotamer of 12), 156.4 (17), 155.8 (rotamer of 17), 148.9 (rotamer of 6), 148.1 (6), 136.83 and 136.76 (5 and its rotamer), 133.6 (4 and its rotamer), 124.3 (rotamer of 2), 123.9 (2), 123.2 (rotamer of 3), 122.5 (3), 119.1 (rotamer of 1), 118.0 (1), 94.4 (8), 93.7 (rotamer of 8), 89.3 (rotamer of 9), 88.3 (9), 82.4 (rotamer of 18), 81.9 (18), 62.6 (13), 62.3 (rotamer of 13), 61.6 (11), 61.4 (rotamer of 11), 46.3 (10), 44.2 (rotamer of 10), 41.7 (rotamer of 7), 41.2 (7), 29.6 (rotamer of 19), 29.3 (19), 15.6 (14), 15.5 (rotamer of 14), 8.0 (16), 7.5 (15); HRMS (MS ES+, Na) calcd, for C25H40N2O5SiCl: 511.2395, found: 511.2387, Δ=1.6 ppm. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With triethylamine In tetrahydrofuran; methanol; chloroform; ethyl acetate | 19 EXAMPLE 19 EXAMPLE 19 In tetrahydrofuran (50 ml) were dissolved benzyl 2-amino-2-deoxy-4,6-O-isopropylidene-α-D-glucopyranoside (8.1 g, 26.2 mmol), S-t-butyloxycarbonyl-4,6-dimethyl-2-mercaptopyrimidine (7.54 g, 31.4 mmol) and triethylamine (2.2 ml), and the reaction is carried out at room temperature for 24 hours and further in an oil bath at 60° C. for 15 hours. After evaporation, the residue was dissolved in ethyl acetate (150 ml). The solution was washed with cold 0.3 N hydrochloric acid and then water, dried over anhydrous sodium sulfate, and evaporated. The residue was purified by silica gel (200 g) column chromatography (column size: 4*25 cm). The column was washed with a 99:1 (v/v) mixture of chloroform and methanol and, then, eluted with a 49:1 (v/v) mixture of chloroform and methanol. The fractions containing the desired product were combined and the solvent was evaporated. The residue was crystallized from ethyl ether-petroleum ether to give 8.03 g of benzyl 2-t-butyloxycarbonylamino-2-deoxy-4,6-O-isopropylidene-α-D-glucopyranoside, m.p. 69°-70° C., [α]D25 +99.8° (c 0.5, chloroform), Rf1 =0.79, Rf3 =0.65 Elemental analysis for C21 H31 NO7: Calcd.: C, 61.56; H, 7.63; N, 3.42. Found: C, 61.26; H, 7.53; N, 3.77. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
10.I EXAMPLE 10 The resulting hydrochloride was dissolved together with S-t-butyloxycarbonyl-4,6-dimethyl-2-mercaptopyrimidine (1.79 g, 7.44 mmol) and TEA (1.38 ml) in a mixture of water (5 ml) and DMF (5 ml) and the mixture was stirred at room temperature for 20 hours. Water (20 ml) and ether (20 ml) were added to the reaction mixture and the excess S-t-butyloxycarbonyl-4,6-dimethyl-2-mercaptopyridine was extracted. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With hydrogenchloride; triethanolamine; triethylamine In water; N,N-dimethyl-formamide | 5.II EXAMPLE 5 (II) D-glutamic acid γ-methyl ester hydrochloride (19.7 g, 0.1 mol) was dissolved together with triethylamine (hereinafter referred to as TEA; 14 ml) in water (55 ml). To this was added a solution of S-t-butyloxycarbonyl-4,6-dimethyl-2-mercaptopyrimidine (26.4 g, 0.11 mol) in DMF (55 ml) and, TEA (14 ml), and the mixture was stirred at room temperature for 60 hours. Water (200 ml) was then added to the reaction mixture and the mixture was extracted with ether (150 ml*2). The aqueous layer was acidified to pH 2 by adding 3 N hydrochloric acid under ice-cooling, and extracted with ethyl acetate (150 ml*2). The ethyl acetate extracts were combined and washed with 1 N hydrochloric acid and then with water. The extract was dried over anhydrous sodium sulfate and evaporated to obtain oily t-butyloxycarbonyl-D-glutamic acid γ-methyl ester (23.5 g). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With triethanolamine In water; N,N-dimethyl-formamide | 16.I EXAMPLE 16 This ester was dissolved in a mixture of water (5 ml) and DMF (8 ml). To this solution was added TEA (1.84 ml) and s-t-butyloxycarbonyl-4,6-dimethyl-2-mercaptopyrimidine (1.91 g, 7.97 mmol) and the mixture was stirred at room temperature for 20 hours. The purification similar to that described in Example 10 (I) gave t-butyloxycarbonyl-D-glutamic acid γ-isopropyl ester dicyclohexylamine salt (2.5 g). m.p. 131° C. [α]D23 -7.1° (C 0.5, DMF). Rf2 =0.64. Elemental analysis for C25 H46 O6 N2: Calculated: C, 63.80; H, 9.85; N, 5.95. Found: C, 63.57; H, 10.01; N, 6.08. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
71% | In 1,4-dioxane; at 20℃; for 2h; | N,N′ -bis(3-aminoethyl)methylamine (8.9 mL, 69 mmol) was dissolvedin 1,4-dioxane (40 mL) and S-Boc-2-mercapto-4,6-dimethylpyrimidine(4.2 g, 17 mmol) in dioxane (80 mL) was added dropwise to thissolution. The precipitate that formed during the dropwise addition wastaken up in a small amount of water. After stirring for 2 h, the water wasevaporated under reduced pressure. A saturated saline solution (200mL) was added to the residue, followed by extraction with ethyl acetate(50 mL). The organic phase was dried over anhydrous MgSO4 andevaporated under reduced pressure to give 5 as a yellow viscous oil(yield 2.7 g, 12 mmol, 71% yield). MALDI-TOF-MS (positive mode,α-CHCA) m/z = 217.73 (calculated value of C10H23N3O2 + H+ =218.32) (Fig. S5); 1H NMR (500 MHz, CDCl3): δ = 1.44 (9H, s, t-Bu), 1.96(2H, s, NH2CH2), 2.22 (3H, s, CH2N(CH3)CH2), 2.43 (4H, m,NH2CH2CH2N(CH3)CH2CH2NHCO), 2.77 (2H, t, J = 6.0 Hz, NH2CH2),3.20 (2H, d, J = 5.4 Hz, CH2NHCO), and 5.12 (1H, br, CH2NHCO) ppm(Fig. S6). HRMS (EI+) m/z [M]+ Calcd for C10H24N3O2 218.18685,found 218.18729. |
Tags: 41840-28-2 synthesis path| 41840-28-2 SDS| 41840-28-2 COA| 41840-28-2 purity| 41840-28-2 application| 41840-28-2 NMR| 41840-28-2 COA| 41840-28-2 structure
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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 |
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