HRID1953463

反应详情

EQUATION

反应方程式

HRID 1953463 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Zinc powder (6.93 g, 106 mmol) was added to a stirred mixture of 4-(2-benzothiazinylsulfonyl)-3-(N,N-di-t-butoxycarbonylamino)-1-ethyloxycarbonylmethyl-2-pyridinone (3.94 g, 6.48 mmol) and acetic acid (8.73 mL) in ethanol (63 mL). After 16 h, the reaction mixture was filtered and evaporated in vacuo at rt. NCS (0.952 g, 7.13 mmol) was added to a stirred mixture of this residue in methylene chloride (100 mL) at -5° C. After 15 min the reaction was warmed to rt and after a further 40 min the reaction was filtered through celite and evaporated in vacuo to give the title compound contaminated with benzothiazole (1 equivalent) as a yellow solid;

WORKUP

后处理

  1. filtrationthe reaction mixture was filtered
  2. customevaporated in vacuo at rt
  3. filtrationwas filtered through celite
  4. customevaporated in vacuo