反应详情

The product N-pyrazineformyl-L-phenylalanine methyl ester (1.0 g, 3.51 mmol) in Preparation example 2 was dissolved with 10 ml of acetone, 2N NaOH was added dropwise slowly until a pH value of 12˜13 was obtained, and the solution was kept reacting under the condition of ice water bath, the reaction was monitored by TLC and completed after 2 h. Hydrochloric acid was add dropwise under the condition of ice water bath until a pH value of 2˜3 was obtained, a large amount of white solid was produced, the generated precipitate was filtered, washed with water and diethyl ether followed by airing to dry and gave 0.89 g of white product with a yield of 93.6%, m.p.: 166-169° C. 1H-NMR (DMSO-d6, 300 MHz): δ 3.23 (—CH2, m, 2H), 4.74 (—CH, m, 1H), 7.16˜7.25 (-Ph, m, 5H), 8.74 (—CONH, t, 1H), 8.86˜8.89 (-Pyz, t, 2H), 9.14 (-Pyz, d, 1H), 13.06 (—COOH, s, 1H).

1. additionwas added dropwise slowly until a pH value of 12˜13
2. customwas obtained
3. customthe solution was kept reacting under the condition of ice water bath
4. customwas obtained
5. customa large amount of white solid was produced
6. filtrationthe generated precipitate was filtered
7. washwashed with water and diethyl ether
8. customto dry