HRID1446955

反应详情

EQUATION

反应方程式

HRID 1446955 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N-Methyl-N-(2,2-dimethoxyethyl)-2-chloroacetamide (19.5 grams; 0.10 mole), ethylene glycol (6.82 grams; 0.11 mole) and 10 drops of a solution of one gram of p-toluenesulfonic acid in 100 ml of diethyl ether were charged into a glass reaction vessel fitted with a mechanical stirrer, thermometer, distillation head and condenser. The mixture was stirred and heated to about 100° C. to 110° C. Byproduct methanol was distilled off. When no further methanol was evolved, the mixture was cooled to room temperature, sodium carbonate (2 grams) was added and the slurry was stirred for a period of about 1 hour. The slurry was then filtered and the filtrate fractionally distilled under reduced pressure. The desired product N-(1,3-dioxolan-2-ylmethyl)-N-methyl-2-chloroacetamide was obtained as a fraction boiling at 124° C. at 0.30 mm Hg and at 119° C. at 0.15 mm Hg.

WORKUP

后处理

  1. customfitted with a mechanical stirrer
  2. distillationthermometer, distillation head and condenser
  3. temperatureheated to about 100° C. to 110° C
  4. distillationByproduct methanol was distilled off
  5. additionsodium carbonate (2 grams) was added
  6. stirringthe slurry was stirred for a period of about 1 hour
  7. filtrationThe slurry was then filtered
  8. distillationthe filtrate fractionally distilled under reduced pressure