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
8-[Dihydro-furan-(2Z)-ylidenemethanesulfonyl]-2-(4-trifluoromethoxy-phenyl)-2,8-diaza-spiro[4.5]decan-1-one (described in example 213, 15 mg, 0.03 mmol) was dissolved in MeOH (2 mL). The flask was evacuated and then purged with argon. Pd/C (2 mg) was added in one portion and the flask was evacuated, then purged with hydrogen three times. The reaction mixture was then stirred at room temperature for 16 h. The mixture was filtered through Celite® and the filtrate was then concentrated in vacuo and purified by flash column chromatography (3:2 AcOEt/heptane) to give 8-(tetrahydro-furan-2-ylmethanesulfonyl)-2-(4-trifluoromethoxy-phenyl)-2,8-diaza-spiro[4.5]decan-1-one (5 mg, 33%) as a white solid. MS (ESI): 463.3 (MH+).
WORKUP
后处理
- customThe flask was evacuated
- custompurged with argon
- additionPd/C (2 mg) was added in one portion
- customthe flask was evacuated
- custompurged with hydrogen three times
- filtrationThe mixture was filtered through Celite®
- concentrationthe filtrate was then concentrated in vacuo
- custompurified by flash column chromatography (3:2 AcOEt/heptane)