反应详情

A mixture of 4.32 g of 2-bromo-N-[6-(2-bromo-2-methyl-propionyl)-4-trifluoromethyl-6H-pyrazolo[4′,3′:3,4]benzo[1,2-d]thiazol-2-yl]-2-methyl-propionamide, 25 ml of tetrahydrofuran, 10 ml of ethyleneglycol and 1.30 ml of triethylamine was stirred at room temperature for 14 hours. After the completion of the reaction was confirmed by HPLC, water and ethyl acetate were added and then portioned. The ethyl acetate layer was washed with 1M hydrochoric acid, water and brine and dried over magnesium sulfate, filtered, and then concentrated to dryness under reduced pressure. Hexane was added to the residue and the solid was collected by filtration to give 2.87 g (yield: 91%) of 2-bromo-2-methyl-N-(4-trifluoromethyl-6H-pyrazolo[4′,3′:3,4]benzo[1,2-d]thiazol-2-yl)-propionamide as a pale yellow solid.

1. additionwere added
2. washThe ethyl acetate layer was washed with 1M hydrochoric acid, water and brine
3. dry with materialdried over magnesium sulfate
4. filtrationfiltered
5. concentrationconcentrated to dryness under reduced pressure
6. additionHexane was added to the residue
7. filtrationthe solid was collected by filtration