HRID1034955

反应详情

EQUATION

反应方程式

HRID 1034955 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 N-carbobenzyloxypyrrolidine-3-carboxylic acid (10.15 g, 40.72 mmol) and iodomethane (5.08 mL, 81.44 mmol) in N,N′-dimethylformamide (80 mL) was added powdered potassium hydrogen carbonate (8.15 g, 81.44 mmol) and the reaction mixture stirred at ambient temperature for 5 hours. The mixture was partitioned between ethyl acetate and brine and the organic phase washed with water and concentrated. The residue was purified by flash chromatography on silica gel using 5-50% ethyl acetate in hexane to give the title compound (10.59 g, 99%). MS(DCI): m/z 264 (M+H)+.

WORKUP

后处理

  1. customThe mixture was partitioned between ethyl acetate and brine
  2. washthe organic phase washed with water
  3. concentrationconcentrated
  4. customThe residue was purified by flash chromatography on silica gel using 5-50% ethyl acetate in hexane