反应详情

A mixture of 1,2-benzisothiazole-3-carboxylic acid chloride (2.0 g) and 1-(2-methoxyphenyl)-4-(4-amino-2-butynyl)piperazine (2.63 g) in dichloromethane (100 ml), was stirred while triethylamine (2.83 ml) was added dropwise. Stirring was continued overnight. After 24 hr, the reaction mixture was diluted with water and extracted with dichloromethane. The organic phase was dried over anhydrous magnesium sulfate, filtered, and the filtrate was concentrated in vacuo. The residue was chromatographed on silica using ethyl acetate as the eluent. The appropriate fractions were collected and concentrated. The residue was taken up in ether/dichloromethane. Ethereal hydrogen chloride was added. The precipitate was recrystallized from methanol/dichloromethane/ether to provide 2.27 g (45.7%) of product, mp 162°-164° C.

1. additionwas added dropwise
2. waitAfter 24 hr
3. extractionextracted with dichloromethane
4. dry with materialThe organic phase was dried over anhydrous magnesium sulfate
5. filtrationfiltered
6. concentrationthe filtrate was concentrated in vacuo
7. customThe residue was chromatographed on silica
8. customThe appropriate fractions were collected
9. concentrationconcentrated
10. additionEthereal hydrogen chloride was added
11. customThe precipitate was recrystallized from methanol/dichloromethane/ether