HRID1807653
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureat reflux for 4 days
- customThe RM was evaporated
- custompartitioned between saturated aqueous NaHCO3 and DCM
- extractionextracted 3× with DCM
- dry with materialdried over Na2SO4
- customevaporated
- distillationkugelrohr distilled at 10 mbar