反应详情

A solution of 4-amino-α-(aminomethyl)-3,5-dichlorobenzenemethanol (0.56 g,), 2-[2-[[2-[(6-bromohexyl)oxy]ethyl]thio]ethyl]pyridine (0.58 g,) and DEA (0.26 g,) in DMF (10 ml) was stirred under nitrogen for 2 h. The solvent was evaporated in vacuo and the residual oil partitioned between 8% sodium bicarbonate solution (100 ml) and dichloromethane (100 ml). The aqueous phase was re-extracted with dichloromethane (100 ml) and the combined organic phases dried and evaporated in vacuo to give an oil. Purification by FCC eluting with System G (98:2:1) gave an oil. Trituration with hexane afforded the title compound (451 mg,) as a solid m.p. 59.5°-62°. T.l.c. (System E 40:10:1) Rf 0.32.

1. customThe solvent was evaporated in vacuo
2. customthe residual oil partitioned between 8% sodium bicarbonate solution (100 ml) and dichloromethane (100 ml)
3. extractionThe aqueous phase was re-extracted with dichloromethane (100 ml)
4. customthe combined organic phases dried
5. customevaporated in vacuo
6. customto give an oil
7. customPurification by FCC
8. washeluting with System G (98:2:1)
9. customgave an oil