反应详情

To a mixture of 2-phenylaminobenzoxazole-6-acetic acid(0.067 g), methyl 2-methyl-3-(2-methoxy-5-aminophenoxy)butyrate(0.057 g), hydroxybenzotriazole (0.067 g), and N-methylmorpholine(0.05 ml) in dimethylformamide(0.25 ml) was added 1-(3-dimethylaminopropyl)3-ethylcarbodiimide hydrochloride(0.095 g). The resultant mixture was stirred for 48 hrs then added to water and extracted with ethyl acetate. The organic layer was separated, washed with aqueous acetic acid, brine, aqueous sodium bicarbonate (2 times), dried and evaporated to dryness. The residue was purified by purified by chromatography on silica using an increasingly polar mixture of ethyl acetateldichloromethane and the appropriate fraction yielded, after evaporation to dryness, a solid which was triturated with a mixture of diethylether/hexane to give the product (0.08 g) as a purple-pink solid.

1. extractionextracted with ethyl acetate
2. customThe organic layer was separated
3. washwashed with aqueous acetic acid, brine, aqueous sodium bicarbonate (2 times)
4. customdried
5. customevaporated to dryness
6. customThe residue was purified
7. customby purified by chromatography on silica using
8. additionan increasingly polar mixture of ethyl acetateldichloromethane
9. customthe appropriate fraction yielded
10. customafter evaporation to dryness
11. customa solid which was triturated with a mixture of diethylether/hexane