反应详情

1.0 g (1.72 mmol) (E)-2-hydroxy-5-[4-(2-methoxycarbonylvinyl)benzoyloxy]benzoic acid 11-(2-methylacryloyloxy)undecyl ester, 0.37 g (2.24 mmol) 4-propylbenzoic acid and 58 mg (0.47 mmol) 4-dimethylaminopyridine were dissolved in 20 ml of dichloromethane. A suspension of 0.43g (2.24 mmol) N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride and 10 ml dichloromethane were added dropwise in the course of 45 minutes. After 65 hour at room temperature the reaction mixture was partitioned between dichloromethane and water; the organic phase was washed repeatedly with water, dried over sodium sulfate, filtered and concentrated by rotary evaporation. Chromatography of the residue on 120 g silica gel using cyclohexane:ethyl acetate 4:1 and subsequent crystallisation form 50 ml isopropyl alcohol yielded 0.99 g (79%) (E)-5-[4-(2-methoxycarbonylvinyl)benzoyloxy]-2-(4-propylbenzoyloxy)benzoic acid 11-(2-methylacryloyloxy)undecyl ester as white powder, m.p. (C/N) 86.8° C., cl.p (N/I) 102.8° C.

1. additionwere added dropwise in the course of 45 minutes
2. customAfter 65 hour at room temperature the reaction mixture was partitioned between dichloromethane and water
3. washthe organic phase was washed repeatedly with water
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated by rotary evaporation