HRID2357038
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas refluxed for 3 h
- filtrationThe catalyst was filtered
- concentrationthe filtrate concentrated
- custompurified
- customYield
- custommp, 202° C.