HRID129033

反应详情

EQUATION

反应方程式

HRID 129033 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of benzoic acid (14.6 g, 0.12 mol) and citronellol (15.6 g, 0.1 mol) in tetrahydrofuran (THF) was heated on a water bath for 4 hours after the addition of concentrated sulfuric acid. The reaction was monitored by thin layer chromatography (TLC), and when the reaction was over, the reaction mixture was quenched over ice/water, extracted with THF or methylene chloride, washed with 5% sodium hydrogen carbonate, and dried over magnesium sulfate. The reaction mixture was concentrated under vacuum and purified by open column chromatography to yield 4.95 g (yield: 19%) of a product having the following physical properties.

WORKUP

后处理

  1. temperaturewas heated on a water bath for 4 hours
  2. customwas quenched over ice/water
  3. extractionextracted with THF or methylene chloride
  4. washwashed with 5% sodium hydrogen carbonate
  5. dry with materialdried over magnesium sulfate
  6. concentrationThe reaction mixture was concentrated under vacuum
  7. custompurified by open column chromatography