HRID1264583

反应详情

EQUATION

反应方程式

HRID 1264583 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a mixture under nitrogen of 1.5 g (3.53 mmol) of methyl 3-hydroxy-2-[(4-methoxybenzenesulfonyl)-(2-nitrobenzyl)amino]propionate in 5 ml of dry ethanol was added 1.12 g (17.69 mmol) of ammonium formate followed by the addition of 0.50 g of 10% palladium on carbon. The mixture was stirred overnight at room temperature and heated at 80° C. for 2 hours. The mixture was filtered through diatomaceous earth and the filtrate concentrated to dryness under vacuum to give a semisolid. Trituration with ethyl acetate gave 0.65 g (47%) of white crystals, m.p. 138-140° C.; Anal. for C18H22N2O6S: Calc'd: C, 54.8; H, 5.6; N, 7.1; Found: C, 53.0; H, 5.6; N, 6.8.

WORKUP

后处理

  1. temperatureheated at 80° C. for 2 hours
  2. filtrationThe mixture was filtered through diatomaceous earth
  3. concentrationthe filtrate concentrated to dryness under vacuum
  4. customto give a semisolid