HRID504540

反应详情

EQUATION

反应方程式

HRID 504540 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

A mixture of 5-chloro-2-fluoro-benzaldehyde (10 g, 63 mmol), Piperazine-1-carboxylic acid tert-butyl ester (12 g, 63 mmol), K2CO3 (17 g, 123 mmol) in DMF (60 mL) was heated at 150° C. for 2 h. After cooled to room temperature, the mixture was poured into water (300 mL) and partitioned between diethyl ether and water. The combined organic phases were washed with water, dried over anhydrous Na2SO4 and concentrated. The residue was purified by flash column to give the title compound as a yellow solid (9 g).

WORKUP

后处理

  1. temperatureAfter cooled to room temperature
  2. custompartitioned between diethyl ether and water
  3. washThe combined organic phases were washed with water
  4. dry with materialdried over anhydrous Na2SO4
  5. concentrationconcentrated
  6. customThe residue was purified by flash column