反应详情

A mixture of α-[[acetyl[6-[2-(2-pyridinyl)ethoxy]hexyl]amino]methyl]-4-amino-3,5-dichlorobenzenemethanol acetate (ester) (130 mg) in sodium hydroxide (5 ml) and ethanol (5 ml) was stirred at room temperature for 18 h. The mixture was heated under reflux for 20 h, cooled, evaporated in vacuo and the aqueous layer extracted with ethyl acetate (2×20 ml). The combined organic extracts were dried and concentrated to give a yellow oil which was triturated in ether/hexane to give the title compound as a white solid (80 mg) m.p. 92°-95°, t.l.c. (System A 80:20:1) Rf 0.44.

1. temperatureThe mixture was heated
2. temperatureunder reflux for 20 h
3. temperaturecooled
4. customevaporated in vacuo
5. extractionthe aqueous layer extracted with ethyl acetate (2×20 ml)
6. customThe combined organic extracts were dried
7. concentrationconcentrated
8. customto give a yellow oil which
9. customwas triturated in ether/hexane