HRID2357038

反应详情

EQUATION

反应方程式

HRID 2357038 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In an atmosphere of nitrogen 10% Pd—C (1.17 g) was added to a mixture of compound of example 39c (11.7 g; 36.67 mmol) and ammonium formate (11.56 g; 116.23 mmol) in methanol (110 mL) It was refluxed for 3 h. The catalyst was filtered and the filtrate concentrated and purified using flash chromatography (silica gel, 10% CH3CN in chloroform). Yield, 8.3 g (84.2%); mp, 202° C.: MS (ESI−): 228 (M−1); analysis: C9H11NO4S requires C, 47.15; H, 4.84; N, 6.11; S, 13.98; found: C, 47.39; H, 4.72; N, 6.53; S, 13.53%.

WORKUP

后处理

  1. temperaturewas refluxed for 3 h
  2. filtrationThe catalyst was filtered
  3. concentrationthe filtrate concentrated
  4. custompurified
  5. customYield
  6. custommp, 202° C.