HRID496622

反应详情

EQUATION

反应方程式

HRID 496622 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a stirring solution of bromoacetyl bromide (29.8 g, 148 mmol) in THF (250 mL) at 0° C. was added via an addition funnel a solution of Boc-piperazine (25 g, 134 mmol) and triethylamine (14.9 g, 148 mmol) in THF (75 mL). After 1 h, a few grams of ice were added and the mixture was diluted with ethyl acetate and cold water. The layers were separated and the organic phase was washed with 1 M aq. citric acid, brine, satd aq. NaHCO3 and again with brine. The organic phase was then dried with MgSO4, filtered, and concentrated in vacuo to give 38.2 g (93%) of an off-white powder.

WORKUP

后处理

  1. customThe layers were separated
  2. washthe organic phase was washed with 1 M aq. citric acid, brine
  3. dry with materialThe organic phase was then dried with MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo