HRID565600
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 8-benzyl-1-(3-methylphenyl)-1,3,8-triazaspiro[4.5]dec-2-en-4-one (1.64 g, 4.9 mmol) and 10% palladium on charcoal (0.8 g) in a mixture of methanol (100 mL) and methanol saturated with anhydrous hydrochloride gas (5 mL) was shaken in a Parr hydrogenator at 55 psi for 24 h. The resultant mixture was filtered through a plug of Celite, and the filtrate concentrated under vacuum. The residue was subjected to column chromatography on silica gel eluting with a 1:1 mixture of 10% methanol in chloroform and chloroform saturated with ammonia gas. Collection and concentration of appropriate fractions provide the title compound.
WORKUP
后处理
- filtrationThe resultant mixture was filtered through a plug of Celite
- concentrationthe filtrate concentrated under vacuum
- additionThe residue was subjected to column chromatography on silica gel eluting with a 1:1 mixture of 10% methanol in chloroform and chloroform saturated with ammonia gas
- customCollection and concentration of appropriate fractions