HRID1743820
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
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
To a solution of N,N-dibenzyl-N-{[1-(2-methoxy-2-methylpropyl)piperidin-4-yl]methyl}amine (EXAMPLE 4, Step 5, 756 mg, 1.85 mmol) and ammonium formate (583 mg, 9.24 mmol) in methanol (40 mL) and water (15 mL) was added 10% palladium on carbon (185 mg) at ambient temperature. The mixture was heated at 80° C. for 6 h. After cooling, the mixture was filtered through a pad of Celite and the filtrate was concentrated in vacuo. The obtained residue was partitioned between dichlorometane and aqueous ammonia. After extraction with dichloromethane, the combined organic extract was dried over magnesium sulfate and concentrated to give 275 mg (66%) of the title compound as a pale yellow oil.
WORKUP
后处理
- temperatureAfter cooling
- filtrationthe mixture was filtered through a pad of Celite
- concentrationthe filtrate was concentrated in vacuo
- customThe obtained residue was partitioned between dichlorometane and aqueous ammonia
- extractionAfter extraction with dichloromethane
- extractionthe combined organic extract
- dry with materialwas dried over magnesium sulfate
- concentrationconcentrated