反应详情

温度

0 °C

To a solution of 5-(4-Chloro-phenyl)-7-trifluoromethyl-3-trimethylsilanylethynyl-pyrazolo[1,5-a]pyrimidine (13.3 g, 34 mmol) in THF (60 mL) and MeOH (150 mL) at 0° C. was added K2CO3 (467 mg, 10 mol %) and the mixture was stirred at 0° C. for 6 h, diluted with TBME and ice water, separated, washed with brine, dried over Na2SO4, concentrated and purified by column chromatography (heptane/EtOAc 100:0-90:10), triturated in heptane, filtered and dried to give the title compound (5.0 g, 45%) as an orange crystalline solid. MS (ISP) 322.2 [(M+H)+] and 324.2 [(M+2+H)+]; mp 102-103° C.

1. customseparated
2. washwashed with brine
3. dry with materialdried over Na2SO4
4. concentrationconcentrated
5. custompurified by column chromatography (heptane/EtOAc 100:0-90:10)
6. customtriturated in heptane
7. filtrationfiltered
8. customdried