反应详情

Acetic anhydride (132 mg) in pyridine (2 ml) was added dropwise to a solution of 4-amino-3,5-dichloro-α-[[[6-[2-(2-pyridinyl)ethoxy]hexyl]amino]methyl]benzenemethanol (250 mg) in pyridine (2 ml). The solution was stirred under nitrogen at room temperature overnight and more acetic anhydride (66 mg) in pyridine was added. After stirring for a further 12 h, the solution was evaporated in vacuo to give an oil which was partioned between water (5 ml) and ether (5 ml). The aqueous layer was re-extracted with ether (5 ml) and the combined organic layers were dried and concentrated to give the title compound as a clear oil (190 mg), t.l.c. (System A 80:20:1) Rf 0.5.

1. stirringAfter stirring for a further 12 h
2. customthe solution was evaporated in vacuo
3. customto give an oil which
4. extractionThe aqueous layer was re-extracted with ether (5 ml)
5. customthe combined organic layers were dried
6. concentrationconcentrated