HRID661253
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- washthe organic phase was washed with aqueous 1 N hydrochloric acid solution
- dry with materialdried (magnesium sulphate)
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customThis gave 550 mg of crude product in 80% purity (LC-MS), which was reacted without any further purification steps