反应 #4221

反应方程式

dimethyl sulphide

dimethyl sulphate

1-(4-chlorophenoxy)-3,3-dimethyl-butan-2-one

sodium methylate

→

2-(4-chlorophenoxymethyl)-2-tert.-butyl-oxirane

收率 84.0%

溶剂

acetonitrile

acetonitrile

acetonitrile

反应条件

后处理

1. 1
   workup.STIRRINGThe mixture was stirred for 30 minutes
2. 2
   workup.WAITThe reaction mixture was subsequently stirred overnight
3. 3
   浓缩It was then concentrated
4. 4
   其他the residue was partitioned between water and ethyl acetate
5. 5
   其他the organic phase was separated off
6. 6
   洗涤washed twice with water and once with saturated sodium chloride solution
7. 7
   干燥dried over sodium sulphate
8. 8
   浓缩concentrated
9. 9
   workup.DISTILLATIONthe residue was distilled in vacuo

实验过程

A solution of 162 ml (2.2 moles) of dimethyl sulphide in 400 ml of absolute acetonitrile was added to a solution of 189 ml (2.0 moles) of dimethyl sulphate in 1,200 ml of absolute acetonitrile at room temperature. The reaction mixture was stirred overnight at room temperature. 118.8 g (2.2 moles) of sodium methylate were then added. The mixture was stirred for 30 minutes and a solution of 272 g (1.2 moles) of 1-(4-chlorophenoxy)-3,3-dimethyl-butan-2-one in 600 ml of absolute acetonitrile was then added dropwise in the course of 30 minutes. The reaction mixture was subsequently stirred overnight. It was then concentrated, the residue was partitioned between water and ethyl acetate, the organic phase was separated off, washed twice with water and once with saturated sodium chloride solution, dried over sodium sulphate and concentrated and the residue was distilled in vacuo. 242.4 g (84% of theory) of 2-(4-chlorophenoxymethyl)-2-tert.-butyl-oxirane of boiling point 115°-22° C./0.003 mm Hg column and of melting point 50°-52° C. were obtained.

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