反应详情

10.0 g (41 mmol) of methyl 2-(4'-hydroxymethylphenyl)benzoate was dissolved in 7.9 g of pyridine and n-hexane (100 ml). 8.3 g (31 mmol) of phosphorus tribromide was dropwise added thereto under cooling with ice, followed by stirring for 2 hours as such. The reaction liquid was added to an aqueous solution of sodium hydrogencarbonate, followed by the extraction with n-hexane. The organic phase was washed with water, dried and subjected to vacuum concentration. The residue was purified by silica gel column chromatography (a n-hexane/ethyl acetate system) to give 9.5 g of the title compound (yield 75%).

1. temperatureunder cooling with ice
2. customThe reaction liquid
3. extractionfollowed by the extraction with n-hexane
4. washThe organic phase was washed with water
5. customdried
6. concentrationsubjected to vacuum concentration
7. customThe residue was purified by silica gel column chromatography (a n-hexane/ethyl acetate system)