反应详情

温度

100 °C

To 5 ml of N,N-dimethylformamide were dissolved 0.68 g (3.0 mmol) of 6,6-difluoro-5-methyl-5-hexenyl methanesulfonate and 0.24 g (1.5 mmol) of 1H-benzoimidazole-5-carboxylic acid, followed by the addition of 0.42 g (5.0 mmol) of sodium hydrogencarbonate and stirring at 100° C. for 3 hours. The reaction liquid was then poured in water and extracted with ethyl acetate. The organic layer was washed with water and a saturated saline solution in this order, followed by drying over anhydrous magnesium sulfate and concentration under reduced pressure. The residue was purified with silica gel column chromatography (ethyl acetate:hexane 1:2) to obtain 0.22 g (yield: 35%) of 6,6-difluoro-5-methyl-5-hexenyl 1-(6,6-difluoro-5-methyl-5-hexenyl)-1H-benzoimidazole-5-carboxylate as the first elution component and 0.21 g (yield: 33%) of 6,6-difluoro-5-methyl-5-hexenyl 3-(6,6-difluoro-5-methyl-5-hexenyl)-3H-benzoimidazole-5-carboxylate as the second elution component.

1. customThe reaction liquid
2. extractionextracted with ethyl acetate
3. washThe organic layer was washed with water
4. dry with materialby drying over anhydrous magnesium sulfate and concentration under reduced pressure
5. customThe residue was purified with silica gel column chromatography (ethyl acetate:hexane 1:2)