HRID1285556

反应详情

EQUATION

反应方程式

HRID 1285556 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred mixture of 10.6 g of 2-nitro-2-azapropanol and 25 ml of dichloromethane under a nitrogen atmosphere was added dropwise and with ice-cooling 12 g of acetyl chloride. The cooling bath was removed and the mixture was slowly heated to reflux. After 3 hours the solution was allowed to cool and was then triturated with 50 ml of ice water. The organic phase was separated, dried (MG SO4), and distilled. The product 2-nitro-2-azapropyl acetate had b.p. 56°-57° C. at 0.07 mm Hg.

WORKUP

后处理

  1. additionwas added dropwise and with ice-
  2. customThe cooling bath was removed
  3. temperaturethe mixture was slowly heated to reflux
  4. temperatureto cool
  5. customwas then triturated with 50 ml of ice water
  6. customThe organic phase was separated
  7. customdried (MG SO4)
  8. distillationdistilled