反应 #158338

反应方程式

2-(3,4-dichlorophenyl)-7-[3-methoxy-4-(3-methyl-1H-1,2,4-triazol-1-yl)phenyl]hept-6-yn-2-ol

trimethylsilylazide

toluene

→

title compound

7-(3,4-dichlorophenyl)-3-[3-methoxy-4-(3-methyl-1H-1,2,4-triazol-1-yl)phenyl]-7-methyl-4,5,6,7-tetrahydro[1,2,3]triazolo[1,5-a]pyridine

溶剂

ethyl acetate

反应条件

后处理

1. 1
   温度cooling
2. 2
   温度to cool to room temperature
3. 3
   洗涤the mixture was washed with saturated aqueous sodium hydrogen carbonate solution and saturated brine
4. 4
   干燥dried over anhydrous sodium sulfate
5. 5
   其他the solvent was evaporated under reduced pressure
6. 6
   其他The residue was purified by silica gel column chromatography (ethyl acetate/hexane)

实验过程

Boron trifluoride-diethyl ether complex (75.3 μL) was added to a mixture of 2-(3,4-dichlorophenyl)-7-[3-methoxy-4-(3-methyl-1H-1,2,4-triazol-1-yl)phenyl]hept-6-yn-2-ol (88.0 mg), trimethylsilylazide (105 μL) and toluene (4 mL) under ice-cooling, and the mixture was stirred at room temperature for 30 min, at 70° C. for 15 min and at 110° C. for 6 hr, and allowed to cool to room temperature. The reaction mixture was diluted with ethyl acetate, the mixture was washed with saturated aqueous sodium hydrogen carbonate solution and saturated brine, and dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (15.7 mg).

来源