HRID2300164

反应详情

EQUATION

反应方程式

HRID 2300164 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. filtrationThe catalyst was filtered off from the reaction solution, 1.3 g of palladium carbon
  2. additionwas added
  3. filtrationThe catalyst was filtered off from the reaction solution, 2.6 g of palladium carbon
  4. additionwas added
  5. stirringthe solution was stirred overnight in a hydrogen atmosphere at 4.2 atmospheric pressure
  6. filtrationThe catalyst was filtered off from the reaction solution
  7. customthe solvent was evaporated
  8. customthe resulting residue was purified by silica gel column chromatography (ethyl acetate/methanol)