HRID275285

反应详情

EQUATION

反应方程式

HRID 275285 的结构方程式

CONDITIONS

反应条件

温度
55 °C

PROCEDURE

实验过程

To a solution of the compound of Reference Example 16 (78.8 g) in ethanol (1.5 ) was added pyridinium p-toluenesulfonate (8.04 g) and the mixture was stirred at 55° C. for 4 hours. To this reaction mixture was added 1N-NaOH (ca. 30 ml) and the solvent was distilled off under reduced pressure. To the residue was added ether (300 ml) and the suspension was dried over anhydrous sodium sulfate. The insolubles were filtered off and the filtrate was concentrated under reduced pressure. The residue was subjected to vacuum distillation to give 42.4 g of 2-[(tetrahydropyran-2-yl)thio]ethanol. bp 93°-94° C. /0.2 mmHg

WORKUP

后处理

  1. distillationthe solvent was distilled off under reduced pressure
  2. additionTo the residue was added ether (300 ml)
  3. dry with materialthe suspension was dried over anhydrous sodium sulfate
  4. filtrationThe insolubles were filtered off
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. distillationThe residue was subjected to vacuum distillation