HRID661253

反应详情

EQUATION

反应方程式

HRID 661253 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

651 mg (1.38 mmol) of the compound from Example 83A, 0.99 g (9.69 mmol) of thiomorpholine and 0.84 ml (0.63 g, 4.84 mmol) of N,N-diisopropylethylamine were added to 9 ml of 1-methyl-2-pyrrolidone and heated in a single-mode microwave (Emrys Optimizer) at 150° C. for 1 h. For workup, the reaction solution was admixed with water. After addition of ethyl acetate and phase separation, the organic phase was washed with aqueous 1 N hydrochloric acid solution, dried (magnesium sulphate), filtered and concentrated under reduced pressure. This gave 550 mg of crude product in 80% purity (LC-MS), which was reacted without any further purification steps.

WORKUP

后处理

  1. washthe organic phase was washed with aqueous 1 N hydrochloric acid solution
  2. dry with materialdried (magnesium sulphate)
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. customThis gave 550 mg of crude product in 80% purity (LC-MS), which was reacted without any further purification steps