HRID711974
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
A mixture of {trans-4-[(6-nitrothieno[3,2-b]pyridin-7-yl)amino]cyclohexyl}acetonitrile (1.0 g, 3.2 mmol) and 10% palladium on carbon (0.3 g, 0.3 mmol) in methanol (30 mL) was hydrogenated under balloon pressure of H2 at room temperature for 5 h. The reaction mixture was filtered. The filtrate was concentrated, diluted with dichlormethane, dried over MgSO4, and concentrated. The residue was purified on silica gel (eluting with 0 to 5% MeOH in dichloromethane) to give the desired product. (0.63 g, 70%). LCMS calculated for C15H19N4S (M+H)+: m/z=287.1. Found: 287.1.
WORKUP
后处理
- filtrationThe reaction mixture was filtered
- concentrationThe filtrate was concentrated
- additiondiluted with dichlormethane
- dry with materialdried over MgSO4
- concentrationconcentrated
- customThe residue was purified on silica gel (eluting with 0 to 5% MeOH in dichloromethane)