反应详情

A solution of (a) (6.4 g, 30 mmol) and ethanol (2.1 ml, 40 mmol) in chloroform (60 ml) was saturated with gaseous hydrochloric acid at 0° C. for 0.5 hours. The mixture was left 20 hours at 4° C. then concentrated in vacuo to afford a white foam. This was suspended in chloroform (60 ml), treated with 3-fluorophenylenediamine (3.8 g, 30 mmol) and heated under reflux for 1 hour. The mixture was poured onto water. The aqueous phase was then basified with sodium bicarbonate and extracted three times with dichloromethane. The organic extract was washed with water, brine, dried over magnesium sulfate and evaporated. The resulting residue was triturated with ethyl acetate, then diethyl ether to give a white solid (5.2 g, 55%).

1. concentrationthen concentrated in vacuo
2. customto afford a white foam
3. temperatureheated
4. temperatureunder reflux for 1 hour
5. additionThe mixture was poured onto water
6. extractionextracted three times with dichloromethane
7. extractionThe organic extract
8. washwas washed with water, brine
9. dry with materialdried over magnesium sulfate
10. customevaporated
11. customThe resulting residue was triturated with ethyl acetate