HRID262355

反应详情

EQUATION

反应方程式

HRID 262355 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a 2-liter flask fitted with a reflux condenser, a water separator and a stirrer is charged 265 g of 2,6,6-trimethylcyclohex-2-en-1,4-dione (prepared by the method described in Helv. Chim. Acta, 39:2041 [1956]), 266 g of propylene glycol, 500 ml of benzene and 1 g of p-toluenesulfonic acid. The reactants are stirred and refluxed until no additional water is collected in the water separator. The product is washed with water to a pH of 6, and the solvent is stripped off. The residue is vacuum distilled through a 9" Goodloe column to yield 257 g of product, boiling point 92° C. at 1 mm Hg (80% yield).

WORKUP

后处理

  1. customTo a 2-liter flask fitted with a reflux condenser
  2. customprepared by the method
  3. customis collected in the water separator
  4. washThe product is washed with water to a pH of 6
  5. distillationdistilled through a 9" Goodloe column