HRID1029649

反应详情

EQUATION

反应方程式

HRID 1029649 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of (2R,4R)-1-(tert-butoxycarbonyl)-4-hydroxy-2-methylpyrrolidine (1.92 g) and methanesulfonyl chloride (955 μl) in dichloromethane (30 ml) was added dropwise triethylamine (1.99 ml) at 0° C. After one hour, the reaction mixture was washed in turn with 1N-hydrochloric acid and brine and the organic layer was dried over magnesium sulfate. Evaporation of the solvent gave an oil, which was chromatographed on silica gel (200 ml) eluting with a mixture of hexane and ethyl acetate (1:1, V/V) to give (2R,4R)-1-(tert-butoxycarbonyl)-4-methanesulfonyloxy-2-methylpyrrolidine (2.49 g).

WORKUP

后处理

  1. washthe reaction mixture was washed in turn with 1N-hydrochloric acid and brine
  2. dry with materialthe organic layer was dried over magnesium sulfate
  3. customEvaporation of the solvent
  4. customgave an oil, which
  5. customwas chromatographed on silica gel (200 ml)
  6. washeluting with a mixture of hexane and ethyl acetate (1:1, V/V)