HRID82170

反应详情

EQUATION

反应方程式

HRID 82170 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Potassium carbonate (7.67 g, 55.56 mmol) was added to 3-cyclopropyl-1H-pyrazole (2.0 g, 18.52 mmol) in dry DMF (20 mL) at 25° C. and the mixture was stirred for 20 minutes. Ethyl bromoacetate (2.06 mL, 18.52 mmol) was added then the mixture was stirred for 2 days at room temperature. The reaction mixture was neutralized with aqueous HCl (1.0 M), extracted with ether (40 mL) and the organic extract was washed with brine (30 mL), dried over sodium sulfate then evaporated in vacuo. The residue was purified by column chromatography on silica gel (hexane:EtOAc 88:12) to afford the title compound as a yellow oil in 42% yield, 1.50 g.

WORKUP

后处理

  1. stirringthe mixture was stirred for 2 days at room temperature
  2. extractionextracted with ether (40 mL)
  3. extractionthe organic extract
  4. washwas washed with brine (30 mL)
  5. dry with materialdried over sodium sulfate
  6. customthen evaporated in vacuo
  7. customThe residue was purified by column chromatography on silica gel (hexane:EtOAc 88:12)