反应详情

温度

140 °C

A mixture of 5-[3,6-dihydro-3-methyl-2,6-dioxo-4-(trifluoromethyl)-1(2H)-pyrimidinyl]-α,α-dimethyl-1,2-benzisothiazole-3-acetic acid (2.00 g, 0.00484 mol) and quinoline (20.0 ml) is heated to 140° C. with stirring. After 15 minutes, the mixture is cooled to room temperature, diluted with ethyl acetate, washed sequentially with 2 N hydrochloric acid, saturated sodium bicarbonate and brine, dried over anhydrous magnesium sulfate, and concentrated in vacuo to a yellow solid. The solid is recrystallized from hexanes:methylene chloride to give the title compound as an off-white solid (0.640 g, 35.8%, mp 139-140° C.) which is identified by NMR and IR spectral analyses.

1. temperaturethe mixture is cooled to room temperature
2. washwashed sequentially with 2 N hydrochloric acid, saturated sodium bicarbonate and brine
3. dry with materialdried over anhydrous magnesium sulfate
4. concentrationconcentrated in vacuo to a yellow solid
5. customThe solid is recrystallized from hexanes