HRID83814

反应详情

EQUATION

反应方程式

HRID 83814 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

[4-(2-Benzyloxyacetylamino)phenoxy]acetic acid methyl ester 49 (25 g, 76 mmol) was dissolved in methanol (450 ml) in a pressure vessel. Palladium on carbon (5%, 10 g) was added and the mixture stirred under a hydrogen atmosphere (2 kg) for 5 hrs. Catalyst was removed by filtration and methanol distilled off. Crude 50 was recrystal-lised in chloroform:hexane (1:6) to give pure 50 (14 g) as a white powder with an m.p. between 147.5-150° C. IH NMR (CDCl3+DMSO-d6): δ 3.74 (s, 3H, ester), 3.96 (d, 2H, CH2OH), 4.64 (s, 2H, OCH2), 5.48 (t, 1H, OH), 6.80 (d, 2H, Ar), 7.54 (d, 2H, Ar) 9.2 (bs, 1H, NH)

WORKUP

后处理

  1. customCatalyst was removed by filtration and methanol
  2. distillationdistilled off