HRID21400

反应详情

EQUATION

反应方程式

HRID 21400 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture containing 3-(R)-(1-cyano-1,1-diphenylmethyl)piperidine (0.3 g), 2-phenoxyethyl bromide (0.24 g--commercially available), anhydrous potassium carbonate (0.5 g) and acetonitrile (15 ml) was heated under reflux for 5 hours. The mixture was then partitioned between dichloromethane (30 ml) and 10% aqueous potassium carbonate (30 ml), the layers separated, and the aqueous layer extracted with dichloromethane (2×20 ml). The combined dichloromethane extracts were dried (MgSO4) and concentrated in vacuo to give a gum which was purified by column chromatography on silica eluting with dichloromethane containing methanol (0% up to 2%). The product-containing fractions were combined and concentrated in vacuo to give the title compound as a gum, yield 0.254 g.

WORKUP

后处理

  1. temperatureunder reflux for 5 hours
  2. customThe mixture was then partitioned between dichloromethane (30 ml) and 10% aqueous potassium carbonate (30 ml)
  3. customthe layers separated
  4. extractionthe aqueous layer extracted with dichloromethane (2×20 ml)
  5. dry with materialThe combined dichloromethane extracts were dried (MgSO4)
  6. concentrationconcentrated in vacuo
  7. customto give a gum which
  8. customwas purified by column chromatography on silica eluting with dichloromethane
  9. additioncontaining methanol (0% up to 2%)
  10. concentrationconcentrated in vacuo