HRID1600902

反应详情

EQUATION

反应方程式

HRID 1600902 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 4'-(2-propenyl)biphenyl4-ol (1.22 g; Biochemistry 1987, 26(18), 5908) in ethanol (10 ml) at room temperature was treated with a solution of sodium hydroxide (0.215 g) in water (5 ml) and was then heated at reflux. A solution of (±)-α-(chloromethyl)-3-pyridinepropanol (1.0 g) in ethanol (5 ml) was added to the latter and the resulting mixture heated at reflux for 2 hours. The reaction mixture was cooled and then concentrated under reduced pressure. The residue was purified by column chromatography over silica eluting with dichloromethane:ethanol (95:5) to give a solid. Trituration with diethyl ether:methanol (9:1) gave the title compound as a colourless solid (0.256 g).

WORKUP

后处理

  1. temperaturewas then heated
  2. temperatureat reflux
  3. temperaturethe resulting mixture heated
  4. temperatureat reflux for 2 hours
  5. temperatureThe reaction mixture was cooled
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by column chromatography over silica eluting with dichloromethane:ethanol (95:5)
  8. customto give a solid