反应详情

Benzyl 5-hydroxymethyl-2-methoxybenzoate (Patent Application No. Hei 11-162235) (15.5 g, 56.9 mmol) and 300 ml of dehydrated ether were mixed and phosphorus tribromide (2.0 ml, 21.1 mmol) was added dropwise under stirring and cooling with ice, which was further stirred for 1 hour. Ice water was added to the reaction mixture and ether layer was separated. The ether layer was washed with water, saturated sodium hydrogencarbonate and brine in sequence, then dried over anhydrous sodium sulfate and concentrated. The crystals obtained were recrystallized from diisopropyl ether to obtain 12.7 g (66%) of the aimed compound as colorless prisms.

1. temperaturecooling with ice, which
2. stirringwas further stirred for 1 hour
3. customwas separated
4. washThe ether layer was washed with water, saturated sodium hydrogencarbonate and brine in sequence
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationconcentrated
7. customThe crystals obtained
8. customwere recrystallized from diisopropyl ether