HRID582013

反应详情

EQUATION

反应方程式

HRID 582013 的结构方程式

PROCEDURE

实验过程

The title compound was prepared from 2-cyano-3-methylthio-3-(4-tolyl) acrylamide (232 mg, 1.0 mmol), 4-methoxyphenylhydrazine hydrochloride (192 mg, 1.1 mmol) and sodium hydroxide (44 mg, 1.1 mmol) following the procedure used for the compound of Example 12. The crude product was purified by chromatography (SiO2, 75% ethyl acetate in hexane) and recrystallisation from ethyl acetate-hexane to give the title compound as white crystals (101 mg) m.p. 174-175°. δH (d6DMSO) 7.49-7.43 (4H, m), 7.28 (2H, d, J 7.8 Hz), 7.07 (2H, d, J 8.9 Hz), 6.32 (2H, br s), 3.81 (3H, s) and 2.29 (3H, s), one set of amino protons not observed. MS (ES+) 323 (MH+, 100%).

WORKUP

后处理

  1. customThe crude product was purified by chromatography (SiO2, 75% ethyl acetate in hexane) and recrystallisation from ethyl acetate-hexane