反应详情

6.81 g (0.03 mol) of 3-difluoromethoxy-benzyl bromide and 6.27 g (0.03 mol) of 2,2-dimethyl-3-(2',2'-dichlorovinyl)-cyclopropanecarboxylic acid were dissolved in 150 ml of toluene, 0.5 g of tetrabutylammonium bromide and 2 g of powdered KOH (industrial product, 87% pure) were added and the mixture was heated to the boil for 2-3 hours. After cooling, the reaction mixture was poured into 150 ml of water, the toluene phase was separated off, washed with 100 ml of water and dried with sodium sulphate and the toluene was distilled off in vacuo. Last residues of solvent were removed by incipient distillation at a bath temperature of 60°-80° C./0.2 to 1 mm Hg. 8.3 g (78% of theory) of 3-difluoromethoxy-benzyl 2,2-dimethyl-3-(2',2'-dichlorovinyl)-cyclopropanecarboxylate were obtained as a viscous oil with the refractive index hD20 =1.5110.

1. temperaturethe mixture was heated to the boil for 2-3 hours
2. temperatureAfter cooling
3. customthe toluene phase was separated off
4. washwashed with 100 ml of water
5. dry with materialdried with sodium sulphate
6. distillationthe toluene was distilled off in vacuo
7. customLast residues of solvent were removed by incipient distillation at a bath temperature of 60°-80° C./0.2 to 1 mm Hg