HRID1511850
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
To a suspension of palladium hydroxide on carbon (0.583 g, 0.830 mmol) in MeOH (250 mL) was added a solution of (5R,7R)-7-(4-(3-(benzyloxy)prop-1-ynyl)phenyl)-3-oxa-1-azaspiro[4.4]nonan-2-one (20 g, 41.5 mmol) in MeOH (10 mL). Hydrogen was bubbled through the solution for about 10 minutes and an atmosphere of hydrogen was maintained via balloon. After about 15 hours the reaction mixture was filtered through Celite® and concentrated in vacuo. The crude product was purified by chromatography on silica gel (EtOAc/DCM) to provide (5R,7R)-7-(4-(3-hydroxypropyl)phenyl)-3-oxa-1-azaspiro[4.4]nonan-2-one (5.2 g, 18.89 mmol, 45.5% yield) as a colorless solid.
WORKUP
后处理
- customHydrogen was bubbled through the solution for about 10 minutes
- temperaturean atmosphere of hydrogen was maintained via balloon
- filtrationAfter about 15 hours the reaction mixture was filtered through Celite®
- concentrationconcentrated in vacuo
- customThe crude product was purified by chromatography on silica gel (EtOAc/DCM)