HRID856108

反应详情

EQUATION

反应方程式

HRID 856108 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of tert-butyl 4-(4-acetoxybenzoyl)piperazine-1-carboxylate (18.5 g, 53.1 mmol) prepared in Reference Example 195 and potassium carbonate (370 mg, 2.65 mmol) in methanol (200 ml) was stirred at room temperature overnight. The reaction mixture was concentrated under reduced pressure, 5% hydrochloric acid and methylene chloride were added to the residue, and the mixture was vigorously stirred. The resulting precipitates were collected by filtration, and washed with water and methylene chloride, and then dried in vacuo to afford tert-butyl 4-(4-hydroxybenzoyl)piperazine-1-carboxylate (14.9 g, yield 92%) as a white powder.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated under reduced pressure, 5% hydrochloric acid and methylene chloride
  2. additionwere added to the residue
  3. stirringthe mixture was vigorously stirred
  4. customThe resulting precipitates
  5. filtrationwere collected by filtration
  6. washwashed with water and methylene chloride
  7. customdried in vacuo