反应详情

A mixture of 1,2-benzisothiazole-3-carboxylic acid chloride (1.77 g) and Z-1-(2-methoxyphenyl)-4-(4-amino-2-butenyl)piperazine (2.34 g) in dichloromethane (100 ml) was stirred while triethylamine (2.51 ml) was added dropwise. Stirring was continued overnight. After 24 hr, the reaction mixture was diluted with water and saturated aqueous sodium carbonate solution and extracted with dichloromethane. The organic phase was washed with water, dried over anhydrous magnesium sulfate, filtered, and the filtrate was concentrated in vacuo. The residue was taken up in dichloromethane/ether and hydrogen chloride in ether was added. The precipitate was recrystallized from methanol/dichloromethane/ether to provide 2.31 g (51.7%) of product, mp 184-187.

1. additionwas added dropwise
2. waitAfter 24 hr
3. extractionextracted with dichloromethane
4. washThe organic phase was washed with water
5. dry with materialdried over anhydrous magnesium sulfate
6. filtrationfiltered
7. concentrationthe filtrate was concentrated in vacuo
8. additionhydrogen chloride in ether was added
9. customThe precipitate was recrystallized from methanol/dichloromethane/ether