反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of 13.5 parts of 2-bromo-1-(2,4-dichlorophenyl)ethanone, 5.5 parts of trimethoxymethane, 2 parts of 4-methylbenzenesulfonic acid and 80 parts of methanol is stirred and refluxed overnight (CaCl2 -tube). The reaction mixture is cooled and stirred for 30 minutes with 15 parts of a sodium hydroxide solution 50%. Then there are added 140 parts of 1,1'-oxybisethane and the mixture is washed with 300 parts of water. The organic phase is stirred with silica gel. The latter is filtered off and the filtrate is evaporated. The residue is dissolved in petroleumether. The solution is dried, filtered and evaporated, yielding 14.5 parts (92%) of 1-(2-bromo-1,1-dimethoxyethyl)-2,4-dichlorobenzene as a residue.
WORKUP
后处理
- temperatureThe reaction mixture is cooled
- washthe mixture is washed with 300 parts of water
- stirringThe organic phase is stirred with silica gel
- filtrationThe latter is filtered off
- customthe filtrate is evaporated
- dissolutionThe residue is dissolved in petroleumether
- customThe solution is dried
- filtrationfiltered
- customevaporated