4-巯基-4-甲基-2-戊醇

反应条件: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 12.3 g of acetic anhydride and 6.2 g of formic acid was heated at 40° C. for 1 hour. After cooling to 20° C. 1 g of pyridine was added and subsequently, with stirring, 15 g of 4-mercapto-4-methylpentan-2-ol in the course of 10 minutes. The temperature of the reaction mixture slowly rose to 28° C. After standing overnight it was dissolved in diethylether, washed five times with 3% aqueous NaHCO3 solution and then with aqueous NaCl solution to neutral. The ethereal solution was dried over Na2SO4 and concentrated. Distillation of the residue yielded 10.5 g (58%) of 4-mercapto-4-methylpent-2-yl formate, b.p. 30°-32° C./1 mm, nD20 1.4564. After cooling to 20° C in the course of 10 minutes slowly rose to 28° C washed five times with 3% aqueous NaHCO3 solution The ethereal solution was dried over Na2SO4 concentrated Distillation of the residue

反应条件: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 12.3 g of acetic anhydride and 6.2 g of formic acid was heated at 40°C for 1 hour. After cooling to 20°C 1 g of pyridine was added and subsequently, with stirring, 15 g of 4-mercapto-4-methylpentan-2-ol in the course of 10 minutes. The temperature of the reaction mixture slowly rose to 28°C. After standing overnight it was dissolved in diethylether, washed five times with 3% aqueous NaHCO3 solution and then with aqueous NaCl solution to neutral. The ethereal solution was dried over Na2SO4 and concentrated. Distillation of the residue yielded 10.5 g (58%) of 4-mercapto-4-methylpent-2-yl formate, b.p. 30°-32°C/1 mm, nD20 1.4564. was added in the course of 10 minutes slowly rose to 28°C washed five times with 3% aqueous NaHCO3 solution The ethereal solution was dried over Na2SO4 concentrated Distillation of the residue

反应条件: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 12.3 g of acetic anhydride and 6.2 g of formic acid was heated at 40° C. for 1 hour. After cooling to 20° C. 1 g of pyridine was added and subsequently, with stirring, 15 g of 4-mercapto-4-methylpentan-2-ol in the course of 10 minutes. The temperature of the reaction mixture slowly rose to 28° C. After standing overnight it was dissolved in diethylether, washed five times with 3% aqueous NaHCO3 solution and then with aqueous NaCl solution to neutral. The ethereal solution was dried over Na2SO4 and concentrated. Distillation of the residue yielded 10.5 g (58%) of 4-mercapto-4-methylpent-2-yl formate, b.p. 30°-32° C./1 mm, nD20 1.4564. After cooling to 20° C in the course of 10 minutes slowly rose to 28° C washed five times with 3% aqueous NaHCO3 solution The ethereal solution was dried over Na2SO4 concentrated Distillation of the residue

反应条件: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 12.3 g of acetic anhydride and 6.2 g of formic acid was heated at 40°C for 1 hour. After cooling to 20°C 1 g of pyridine was added and subsequently, with stirring, 15 g of 4-mercapto-4-methylpentan-2-ol in the course of 10 minutes. The temperature of the reaction mixture slowly rose to 28°C. After standing overnight it was dissolved in diethylether, washed five times with 3% aqueous NaHCO3 solution and then with aqueous NaCl solution to neutral. The ethereal solution was dried over Na2SO4 and concentrated. Distillation of the residue yielded 10.5 g (58%) of 4-mercapto-4-methylpent-2-yl formate, b.p. 30°-32°C/1 mm, nD20 1.4564. was added in the course of 10 minutes slowly rose to 28°C washed five times with 3% aqueous NaHCO3 solution The ethereal solution was dried over Na2SO4 concentrated Distillation of the residue