反应 #1435740

ord-d113e0255ddd4a95b781dda3acb68082

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度at reflux
  2. 2
    温度After cooling to room temperature the reaction mixture
  3. 3
    洗涤was washed with 20 ml of a 1 M aqueous sodium carbonate solution and 20 ml water
  4. 4
    干燥The combined organic layers were dried over sodium sulfate
  5. 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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07211579B2uspto-grants-2007_05