HRID2371192

反应详情

EQUATION

反应方程式

HRID 2371192 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of N-(3,4-dichlorophenyl)-1-[(3R)-piperidin-3-ylmethyl]piperidine-4-carboxamide (150 mg) and benzaldehyde (0.04 mL) in dichloromethane was added sodium triacetoxyborohydride (103 mg). The reaction mixture was stirred at room temperature for 18 hours. The reaction was incomplete so sodium triacetoxyborohydride (50 mg) was added and the mixture was stirred for 48 hours. The reaction mixture was partitioned between dichloromethane and water and the organic layer was washed with brine. The organic extract was dried over magnesium sulfate and evaporated. The residue was purified by silica column chromatography, eluting with a gradient of 0 to 10% MeOH in dichloromethane to give the title compound as a white solid (28 mg, 15%)

WORKUP

后处理

  1. additionwas added
  2. stirringthe mixture was stirred for 48 hours
  3. customThe reaction mixture was partitioned between dichloromethane and water
  4. washthe organic layer was washed with brine
  5. extractionThe organic extract
  6. dry with materialwas dried over magnesium sulfate
  7. customevaporated
  8. customThe residue was purified by silica column chromatography
  9. washeluting with a gradient of 0 to 10% MeOH in dichloromethane