HRID426146

反应详情

EQUATION

反应方程式

HRID 426146 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Compound (72) (2.89 g) in anhydrous ethanol (30 ml) was stirred with 10% palladium on carbon (300 mg) under an atmosphere of hydrogen. After 6 hr., the mixture was filtered through celite pad and the filtrate was evaporated in vacuo. The residue was purified by silica gel column chromatography (eluent, dichloromethane:methanol (95:5)) to afford 1 g of the title compound as a white solid. m.p. 272-275° C.; 1H NMR (200 MHz, DMSO-d6) δ 1.06 (6H, d, J=7.4 Hz), 2.36 (3H, s), 2.78 (1H, m), 7.33 (1H, s), 7.45 (1H, s), 7.55 (1H, s), 11.05 (1H, s), 11.34 (1H, s); m/z (EI) 285 (M+).

WORKUP

后处理

  1. filtration, the mixture was filtered through celite pad
  2. customthe filtrate was evaporated in vacuo
  3. customThe residue was purified by silica gel column chromatography (eluent, dichloromethane:methanol (95:5))