HRID1925146

反应详情

EQUATION

反应方程式

HRID 1925146 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

Cyclopropanecarboxamide (58.7 g, 690 mmol) in 1,4-Dioxane (1600 ml) was added 2-bromoacetyl bromide (59.9 ml, 690 mmol) at room temperature and stirred for 4 h at 60° C. The reaction mixture was concentrated to dryness. The residue was dissolved in EtOAc and carefully washed with satd. NaHCO3, water then with brine solution, dried over Na2SO4 and concentrated to get N-(2-bromoacetyl)cyclopropanecarboxamide (138 g, 670 mmol, 97% yield) as an off white solid. This material was used without purification. ESI-MS:m/z 208.0 (M+2H)+.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated to dryness
  2. dissolutionThe residue was dissolved in EtOAc
  3. washcarefully washed with satd
  4. dry with materialNaHCO3, water then with brine solution, dried over Na2SO4
  5. concentrationconcentrated