反应详情

To a solution of 5-amino-2-(pyridin-2-yl)pyrimidin-4-ol (10-e) (120 mg, 0.64 mmol) in MeCN (5 ml) were added HATU (254 mg, 0.67 mmol), Et3N (130 mg, 1.28 mmol) and 2,2-diphenylacetic acid (135 mg, 0.64 mmol). The resulting mixture was stirred at room temperature for 1 hour. Then the mixture was diluted with water and followed by extraction with dichloromethane. The organic layer was washed with brine, dried over sodium sulfate and concentrated under vacuum. The residue was purified by prep-HPLC to provide compound 10-1. 1H NMR (DMSO-d6, 300 MHz): δ 12.50 (br, 1H), 9.85 (br, 1H), 8.73 (m, 2H), 8.10 (m, 1H), 8.00 (m, 1H), 7.60 (m, 1H), 7.35 (m, 10H), 5.75 (s, 1H). (M+H)+=383.2.

1. extractionfollowed by extraction with dichloromethane
2. washThe organic layer was washed with brine
3. dry with materialdried over sodium sulfate
4. concentrationconcentrated under vacuum
5. customThe residue was purified by prep-HPLC