HRID1954651

反应详情

EQUATION

反应方程式

HRID 1954651 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a refluxing solution of 750 g (6.58 mol) 5-methyl-2-hexanone in 1.13 1 n-hexane at 65° C., 1.06 kg (7.89 mol) sulfuryl chloride was added over a period of 2 h. After complete addition of the sulfuryl chloride, the reaction mixture was allowed to cool to room temperature, was washed 4 times with 150 ml H2O, dried (MgSO4) and concentrated in vacuo. The residue was distilled over a 5 cm Vigreux-column (80 mbar, 67-76° C.) to give 884 g of 3-chloro-5-methyl-2-hexanone in the form of a yellowish liquid (purity: 88%, impurity: 11% 3,3-dichloro-5-methyl-2-hexanone).

WORKUP

后处理

  1. washwas washed 4 times with 150 ml H2O
  2. dry with materialdried (MgSO4)
  3. concentrationconcentrated in vacuo
  4. distillationThe residue was distilled over a 5 cm Vigreux-column (80 mbar, 67-76° C.)