HRID1487106

反应详情

EQUATION

反应方程式

HRID 1487106 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

A mixture of 3-nitrophenol (4 g, 28.8 mmol), 2-chloro-N-cyclopropylacetamide (4.61 g, 34.5 mmol), K2CO3 (7.95 g, 57.5 mmol) and 18-CROWN-6 (0.228 g, 0.863 mmol) in N,N-Dimethylformamide (30.0 ml) was stirred under N2 atmosphere for 18 hrs at 50° C. After cooling to RT, the reaction mixture was partitioned between EtOAc (250 ml) and water (250 ml). Aq. phase was re-extracted with EtOAc (200 ml). Combined organic layer was washed with brine (100 ml), dried over sodium sulphate and the solvent was evaporated under vacuum. Crude residue was purified by flash chromatography to obtain N-cyclopropyl-2-(3-nitrophenoxy)acetamide (4.21 gm).

WORKUP

后处理

  1. temperatureAfter cooling to RT
  2. customthe reaction mixture was partitioned between EtOAc (250 ml) and water (250 ml)
  3. extractionAq. phase was re-extracted with EtOAc (200 ml)
  4. washCombined organic layer was washed with brine (100 ml)
  5. dry with materialdried over sodium sulphate
  6. customthe solvent was evaporated under vacuum
  7. customCrude residue was purified by flash chromatography