反应详情

To a solution of (S)-methyl 2-(7-chloro-2-(3-chlorophenyl)-5-methylpyrazolo[1,5-a]pyrimidin-6-yl)-2-hydroxyacetate (1.0 g, 2.73 mmol) in CH2Cl2 (100 mL) at room temperature was added tert-butyl acetate (20 mL) followed by perchloric acid (0.282 mL, 3.28 mmol). The reaction mixture was stirred for 16 h at room temperature. The reaction mixture was quenched with water and diluted with ethyl acetate. The organic phase was washed with saturated NaHCO3 and dried over sodium sulfate. The solvent was evaporated. Purification by silica gel chromatography provided the title compound (520 mg, 50%). 1H NMR (400 MHz, CHLOROFORM-d) δ 8.07-8.00 (m, 1H), 7.89 (dt, J=6.7, 1.9 Hz, 1H), 7.48-7.37 (m, 2H), 6.93 (s, 1H), 5.68 (s, 1H), 3.75 (s, 3H), 2.69 (s, 3H), 1.29 (s, 9H).

1. customThe reaction mixture was quenched with water
2. additiondiluted with ethyl acetate
3. washThe organic phase was washed with saturated NaHCO3
4. dry with materialdried over sodium sulfate
5. customThe solvent was evaporated
6. customPurification by silica gel chromatography