HRID1807653

反应详情

EQUATION

反应方程式

HRID 1807653 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

Concentrated HCl (2 ml) was added to a suspension of (S)-2-methyl-pyrrolidine-2-carboxylic acid (2 g) in butan-1-ol (50 ml) which was heated at 60° C. for 18 h then at reflux for 4 days. The RM was evaporated, partitioned between saturated aqueous NaHCO3 and DCM, extracted 3× with DCM, dried over Na2SO4 and evaporated. The isolated oil was then kugelrohr distilled at 10 mbar to give the title compound as a clear colorless oil from the fraction distilling at an oven temperature of 100-120° C.

WORKUP

后处理

  1. temperatureat reflux for 4 days
  2. customThe RM was evaporated
  3. custompartitioned between saturated aqueous NaHCO3 and DCM
  4. extractionextracted 3× with DCM
  5. dry with materialdried over Na2SO4
  6. customevaporated
  7. distillationkugelrohr distilled at 10 mbar