反应详情

Heat a mixture of 22 g of 2-bromo-4,6-dichlorobenzyl bromide, 30 g anhydrous sodium acetate and 80 mL of glacial acetic acid for 18 hr at 100° C. Evaporate the mixture to a dry residue. Treat the residue with 200 mL of ethanol and 200 mL of 2N NaOH. Stir the mixture at reflux for 3 hr. Cool the mixture and concentrate the cooled mixture to 50 mL. Extract the cooled concentrate with Et2O. Dry the extract over anhydrous K2CO3 and evaporate it to a dry residue. Recrystallize the residue from toluene-hexane to give 10 g of 2-bromo-4,6-dichlorobenzyl alcohol, mp 111°-112° C.

1. temperatureHeat
2. customEvaporate the mixture to a dry residue
3. additionTreat the residue with 200 mL of ethanol and 200 mL of 2N NaOH
4. temperatureat reflux for 3 hr
5. temperatureCool the mixture
6. concentrationconcentrate the cooled mixture to 50 mL
7. extractionExtract the cooled
8. concentrationconcentrate with Et2O
9. customDry the
10. extractionextract over anhydrous K2CO3
11. customevaporate it to a dry residue
12. customRecrystallize the residue from toluene-hexane