反应详情

To a solution of 4-hydroxy-2-(pyridin-2-yl)pyrimidine-5-carboxylic acid, 1-1-h (325.5 mg, 1.5 mmol) in MeCN (10 ml) were added HATU (599 mg, 1.51 mmol), Et3N (159 mg, 1.51 mmol) and ethyl methyl(4-(amino(phenyl)methyl)phenyl)phosphinate (2-d′, 433 mg, 1.5 mmol). The resulting mixture was stirred at room temperature for 2 hour. Then it was concentrated under vacuum and the residue was taken into ethyl acetate followed by washing with saturated NH4Cl. The organic layer was dried over sodium sulfate and concentrated under vacuum. The residue was purified by prep-HPLC to provide the product, 2-4, (159 mg, 22%). 1H NMR (CD3OD, 300 MHz,): δ 8.67 (m, 2H), 8.39 (m, 2H), 7.94 (m, 1H), 7.46 (m, 5H), 7.26 (m, 5H), 6.29 (s, 1H), 3.76 (m, 2H), 1.57 (d, 3H).

1. concentrationThen it was concentrated under vacuum
2. washby washing with saturated NH4Cl
3. dry with materialThe organic layer was dried over sodium sulfate
4. concentrationconcentrated under vacuum
5. customThe residue was purified by prep-HPLC
6. customto provide the product, 2-4, (159 mg, 22%)