HRID975697

反应详情

EQUATION

反应方程式

HRID 975697 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of (2R,4R)-1-allyloxycarbonyl-2-(2-azidoethyl)-4-hydroxypyrrolidine (20.0 g) and triethylamine (15.2 ml) in dichloromethane (300 ml) was added methanesulfonyl chloride (7.8 ml) under ice-cooling. After stirring for 1 hour, water was poured into the mixture. The organic layer was separated and the aqueous layer was extracted twice with dichloromethane. The combined organic layer was washed with 1N hydrochloric acid, sat. sodium bicarbonate, water and brine, dried over magnesium sulfate and evaporated under reduced pressure to give (2R,4R)-1-allyloxycarbonyl-2-(2-azidoethyl)-4-methanesulfonyloxypyrrolidine (15.3 g).

WORKUP

后处理

  1. temperaturecooling
  2. customThe organic layer was separated
  3. extractionthe aqueous layer was extracted twice with dichloromethane
  4. washThe combined organic layer was washed with 1N hydrochloric acid, sat. sodium bicarbonate, water and brine
  5. dry with materialdried over magnesium sulfate
  6. customevaporated under reduced pressure