反应 #1435740
ord-d113e0255ddd4a95b781dda3acb68082
反应方程式
反应物
试剂
无
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1温度at reflux
- 2温度After cooling to room temperature the reaction mixture
- 3洗涤was washed with 20 ml of a 1 M aqueous sodium carbonate solution and 20 ml water
- 4干燥The combined organic layers were dried over sodium sulfate
- 5浓缩concentrated in vacuo
实验过程
To a suspension of 1.60 g (5.03 mmol) 4-iodo-6-(4-methyl-piperazin-1-yl)-pyridin-3-ylamine and 975 mg (7.54 mmol) N,N-diisopropyl ethyl amine in 16 ml dichloromethane was added dropwise 1.76 g (5.53 mmol) 2-(3,5-bis-trifluoromethyl-phenyl)-2-methyl-propionyl chloride at 0° C. The reaction mixture was stirred for 2 h at room temperature and 2 h at reflux. After cooling to room temperature the reaction mixture was washed with 20 ml of a 1 M aqueous sodium carbonate solution and 20 ml water. The combined organic layers were dried over sodium sulfate and concentrated in vacuo to give 3.39 g (100%) of the crude title compound as a brown oil.