反应详情

0.50 g (2.6 mmol) of 6H-pyrazolo[4′,3′:3,4]benzo[1,2-d]thiazol-2-ylamine and 1.5 g (7.9 mmol) of α-chlorophenylacetyl chloride were dissolved in 10 ml of tetrahydrofuran, and 1.3 g (12.9 mmol) of triethylamine was added dropwise to the mixture under ice-cooling. After the mixture was allowed to warm to room temperature and was stirred overnight, 10 ml of water was added to the mixture to quench the reaction. The reaction mixture was extracted with 20 ml of ethyl acetate twice, dried over 5 g of anhydrous magnesium sulfate, and then concentrated under reduced pressure. The crude product was purified by silica gel column chromatography (hexane/ethyl acetate=1/1) to give 1.3 g (yield: 100%) of 2-chloro-N-[6-(2-chloro-2-phenylacetyl)-6H-pyrazolo[4′,3′:3,4]benzo[1,2-d]thiazol-2-yl]-2-phenylacetamide.

1. temperaturecooling
2. customto quench
3. customthe reaction
4. extractionThe reaction mixture was extracted with 20 ml of ethyl acetate twice
5. dry with materialdried over 5 g of anhydrous magnesium sulfate
6. concentrationconcentrated under reduced pressure
7. customThe crude product was purified by silica gel column chromatography (hexane/ethyl acetate=1/1)