HRID908600
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 the compound (1.00 g) obtained in Step 5 and 7.5% palladium carbon (1.0 g) in methanol (15 ml) was stirred under a hydrogen atmosphere (5 atm) at room temperature for 4 hr. The reaction mixture was filtered through celite, and concentrated under reduced pressure. 10% Palladium carbon (500 mg) and methanol (15 ml) were added again to the residue, and the mixture was stirred under a hydrogen atmosphere (5 atm) at room temperature for 6 hr. The reaction mixture was filtered through celite, and the filtrate was concentrated under reduced pressure. The residue was purified by column chromatography (3%-5% methanol/chloroform) to give the title compound (688 mg).
WORKUP
后处理
- filtrationThe reaction mixture was filtered through celite
- concentrationconcentrated under reduced pressure
- addition10% Palladium carbon (500 mg) and methanol (15 ml) were added again to the residue
- stirringthe mixture was stirred under a hydrogen atmosphere (5 atm) at room temperature for 6 hr
- filtrationThe reaction mixture was filtered through celite
- concentrationthe filtrate was concentrated under reduced pressure
- customThe residue was purified by column chromatography (3%-5% methanol/chloroform)