反应详情

温度

80 °C

A mixture of 4-[6-[2,3-bis-(phenylmethoxy)phenyl]hexyloxy]-alpha-oxobenzeneacetic acid (0.3 g) in acetic acid (20 mL) containing concentrated hydrochloric acid (5 mL) was stirred at 80° C. for 2.5 hours. The cooled solution was diluted with water (100 mL) and extracted with three portions of ethyl acetate, then the combined extracts were dried (Na2SO4), and evaporated in vacuo. The residual oil was triturated in turn with cyclohexane and carbon tetrachloride to remove non polar impurities, then was crystallized from dichloromethane and recrystallized from dichloromethane-carbon tetrachloride to give 4-[6-(2,3-dihydroxyphenyl)hexyloxy]-alpha-oxobenzeneacetic acid as a colorless solid, mp 127°-130° C.

1. extractionextracted with three portions of ethyl acetate
2. dry with materialthe combined extracts were dried (Na2SO4)
3. customevaporated in vacuo
4. customThe residual oil was triturated in turn with cyclohexane and carbon tetrachloride
5. customto remove non polar impurities
6. customwas crystallized from dichloromethane
7. customrecrystallized from dichloromethane-carbon tetrachloride