HRID2185649

反应详情

EQUATION

反应方程式

HRID 2185649 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

10 g of (R)-1-(phenylmethyl)-3-pyrrolidinol were dissolved in 160 ml of anhydrous toluene. The solution was stirred under a stream of nitrogen, cooled in an ice/ethanol bath and 8.7 ml of triethylamine were added. At a temperature of −5° C. 4,9 ml of a solution of methanesulfonylchloride in 110 ml of anhydrous toluene were added dropwise over 1,5 hours and the reaction mixture was stirred for 1 hour at 0° C. The solid was filtered and washed with ethyl acetate. The filtrate was washed with water, dried and evaporated in vacuo to give 13,9 g of (R)-3-methanesulfonyloxy-1-(phenylmethyl)-pyrrolidine as an almost colourless oil. M.S. (C.I.) (M/Z): 256 [M+H]+.

WORKUP

后处理

  1. temperaturecooled in an ice/ethanol bath
  2. customAt a temperature of −5° C
  3. stirringthe reaction mixture was stirred for 1 hour at 0° C
  4. filtrationThe solid was filtered
  5. washwashed with ethyl acetate
  6. washThe filtrate was washed with water
  7. customdried
  8. customevaporated in vacuo