HRID256413

反应详情

EQUATION

反应方程式

HRID 256413 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 46.5 (0.217 mole) 2-benzyloxybenzyl alcohol (prepared by reaction of 2-hydroxybenzyl alcohol with benzyl chloride in ethanol containing an equimolar amount of potassium t-butoxide at 100° C.) in 100 ml chloroform was added 17.2 g (0.217 mole) pyridine followed by dropwise addition of a solution of 25.8 g (0.217 mole) thionyl chloride in 60 ml chloroform. The resulting mixture was heated at reflux for 1.5 hours, cooled, washed with water, brine and dried (MgSO4). Evaporation of solvent gave 45.8 g crude oil which was distilled in vacuo to yield 40.7 g (81%) of product as a colorless oil, b.p. 141° C.(1 Torr).

WORKUP

后处理

  1. temperatureThe resulting mixture was heated
  2. temperatureat reflux for 1.5 hours
  3. temperaturecooled
  4. washwashed with water, brine
  5. dry with materialdried (MgSO4)
  6. customEvaporation of solvent
  7. customgave 45.8 g crude oil which
  8. distillationwas distilled in vacuo