HRID1178122

反应详情

EQUATION

反应方程式

HRID 1178122 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

K2CO3 (383 mg, 2.8 mmol) and CH3I (236 mg, 1.66 mmol) were added, with vigorous stirring, to a solution of 4-(2-carboxy-benzoyl)-piperazine-1-carboxylic acid tert-butyl ester (371 mg, 1.1 mmol) in DMF (5 mL) and the resulting mixture was stirred at room temperature for 2 hours. The mixture was then diluted with cold water and the product extracted with ethyl acetate. The organic layer was washed with saturated brine solution, dried over sodium sulphate and concentrated under reduced pressure to afford 390 mg of 4-(2-methoxycarbonyl-benzoyl)-piperazine-1-carboxylic acid tert-butyl ester as a yellow oil. LC-MS purity: 92.15%.

WORKUP

后处理

  1. extractionthe product extracted with ethyl acetate
  2. washThe organic layer was washed with saturated brine solution
  3. dry with materialdried over sodium sulphate
  4. concentrationconcentrated under reduced pressure