HRID1743820

反应详情

EQUATION

反应方程式

HRID 1743820 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

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

  1. temperatureAfter cooling
  2. filtrationthe mixture was filtered through a pad of Celite
  3. concentrationthe filtrate was concentrated in vacuo
  4. customThe obtained residue was partitioned between dichlorometane and aqueous ammonia
  5. extractionAfter extraction with dichloromethane
  6. extractionthe combined organic extract
  7. dry with materialwas dried over magnesium sulfate
  8. concentrationconcentrated