HRID1249585

反应详情

EQUATION

反应方程式

HRID 1249585 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of alpha,alpha-bis(3-methoxyphenyl)-4-pyridine-ethanol (63 g) in acetic acid (400 ml) was hydrogenated over platinum oxide (2 g; 100 p.s.i.; 50°). The reaction was stopped after the uptake of the theoretical amount of hydrogen (0.564 mol), then it was filtered to remove the catalyst and the solvent was evaporated under reduced pressure. After the residue was taken up in water (400 ml) and toluene (200 ml), the mixture was heated to reflux and then made basic with 10N sodium hydroxide. The mixture was cooled to 5°, and the resulting solid was collected by filtration, then was washed in turn with water, toluene, toluene-hexane (1:1) and hexane to give, after drying, 62.5 g of alpha,alpha-bis(3-methoxyphenyl)-4-piperidineethanol, mp 111°-113°.

WORKUP

后处理

  1. filtrationit was filtered
  2. customto remove the catalyst
  3. customthe solvent was evaporated under reduced pressure
  4. temperaturetoluene (200 ml), the mixture was heated
  5. temperatureto reflux
  6. temperatureThe mixture was cooled to 5°
  7. filtrationthe resulting solid was collected by filtration
  8. washwas washed in turn with water, toluene, toluene-hexane (1:1) and hexane
  9. customto give
  10. customafter drying