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
6.47 g of tert-butyl 3-(benzyloxy)-1-oxa-8-azaspiro[4.5]decane-8-carboxylate was dissolved in 100 ml tetrahydrofuran, 1.3 g palladium carbon was added thereto, and the mixture was stirred overnight in a hydrogen atmosphere. The catalyst was filtered off from the reaction solution, 1.3 g of palladium carbon was added thereto, and the solution was stirred overnight in a hydrogen atmosphere. The catalyst was filtered off from the reaction solution, 2.6 g of palladium carbon was added thereto, and the solution was stirred overnight in a hydrogen atmosphere at 4.2 atmospheric pressure. The catalyst was filtered off from the reaction solution, the solvent was evaporated, and the resulting residue was purified by silica gel column chromatography (ethyl acetate/methanol) to give 4.27 g of tert-butyl 3-hydroxy-1-oxa-8-azaspiro[4.5]decane-8-carboxylate.
WORKUP
后处理
- filtrationThe catalyst was filtered off from the reaction solution, 1.3 g of palladium carbon
- additionwas added
- filtrationThe catalyst was filtered off from the reaction solution, 2.6 g of palladium carbon
- additionwas added
- stirringthe solution was stirred overnight in a hydrogen atmosphere at 4.2 atmospheric pressure
- filtrationThe catalyst was filtered off from the reaction solution
- customthe solvent was evaporated
- customthe resulting residue was purified by silica gel column chromatography (ethyl acetate/methanol)