己酸甲硫基甲酯

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

实验步骤: In a three-necked 1000 ml. round-bottomed flask fitted with a mechanical stirrer, thermometer and reflux condenser is placed 63.8 g. of hexanoic acid in 200 ml. of acetonitrile. To the stirred mixture is added, at 20°-30° C., 55 g. of triethylamine over a period of 30 minutes. The reaction mixture is stirred at room temperature for an additional 60 minutes. Then is added, at 20°-24° C., 53 g. of chloromethyl methyl sulfide in a few minutes. The reaction mixture is warmed and allowed to reflux for 24 hours. The reaction mixture is cooled to 5°-0° C. and filtered. The solvent is stripped off under vacuum at 12 mm Hg pressure. The residue is taken up in diethyl ether and washed successively with a 10% solution of sodium bicarbonate and with water. The organic layer is dried over anhydrous sodium sulfate. Distillation gives the title ester; b.p. 57°-58° C./2 mm Hg, n20 1.4545. round-bottomed flask fitted with a mechanical stirrer thermometer and reflux condenser To the stirred mixture is added, at 20°-30° C. Then is added, at 20°-24° C. The reaction mixture is warmed to reflux for 24 hours The reaction mixture is cooled to 5°-0° C. filtered washed successively with a 10% solution of sodium bicarbonate and with water The organic layer is dried over anhydrous sodium sulfate Distillation

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

实验步骤: In a three-necked 1000 ml. round-bottomed flask fitted with a mechanical stirrer, thermometer and reflux condenser is placed 63.8 g. of hexanoic acid in 200 ml. of acetonitrile. To the stirred mixture is added, at 20°-30° C., 55 g. of triethylamine over a period of 30 minutes. The reaction mixture is stirred at room temperature for an additional 60 minutes. Then is added, at 20°-24° C., 53 g. of chloromethyl methyl sulfide in a few minutes. The reaction mixture is warmed and allowed to reflux for 24 hours. The reaction mixture is cooled to 5°-0° C. and filtered. The solvent is stripped off under vacuum at 12 mm Hg pressure. The residue is taken up in diethyl ether and washed successively with a 10% solution of sodium bicarbonate and with water. The organic layer is dried over anhydrous sodium sulfate. Distillation gives the title ester; b.p. 57°-58° C./2 mm Hg, nD20 1.4545. round-bottomed flask fitted with a mechanical stirrer thermometer and reflux condenser To the stirred mixture is added, at 20°-30° C. Then is added, at 20°-24° C. The reaction mixture is warmed to reflux for 24 hours The reaction mixture is cooled to 5°-0° C. filtered washed successively with a 10% solution of sodium bicarbonate and with water The organic layer is dried over anhydrous sodium sulfate Distillation