HRID1678997

反应详情

EQUATION

反应方程式

HRID 1678997 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3-methylbenzaldehyde (24.0 g, 0.2 mole), glycerol (18.4 g, 0.2 mole) and 40% sulfuric acid (2.0 ml) in 150 ml of benzene was heated under a Dean-Stark apparatus until no more water was collected (approximately 2.5 hours). The mixture was cooled, neutralized with potassium carbonate, diluted by the addition of 200 ml of ether and the ether solution washed with water (3 × 100 ml). The organic layer was dried over magnesium sulfate and concentrated to give a residue of 25.1 g of the desired 5-hydroxy-2-(3-methylphenyl)-1,3-dioxane nD25 1.5346.

WORKUP

后处理

  1. customwas collected (approximately 2.5 hours)
  2. temperatureThe mixture was cooled
  3. additiondiluted by the addition of 200 ml of ether
  4. washthe ether solution washed with water (3 × 100 ml)
  5. dry with materialThe organic layer was dried over magnesium sulfate
  6. concentrationconcentrated