反应详情

Poured into a solution of 4.43 g of sodium ethylate in 250 cm3 of ethanol is a solution of 3.21 g of 2-amino-5-chloro-3-iodo-N-(1-propylbutyl)benzamide in 120 cm3 of ethanol then 3.3 cm3 of ethyl formate. The reaction mixture is heated under argon at reflux for 16 h. It is then cooled in order to be evaporated using a rotary evaporator under reduced pressure (5 kPa). 200 cm3 of dichloromethane and 150 cm3 of water are added, while stirring, to the concentration residue. The aqueous phase is extracted with 50 cm3 of dichloromethane. The organic phases are combined, washed with 50 cm3 of a saturated aqueous solution of sodium chloride, dried over sodium sulfate and concentrated using a rotary evaporator under reduced pressure (5 kPa). The ochre product obtained is purified by flash chromatography over silica (column: 200 g; particle size: 15-40 μm; eluent: 100% dichloromethane). After concentrating the fractions under reduced pressure, 2.09 g of 6-chloro-8-iodo-3-(1-propylbutyl)quinazolin-4(3H)-one are obtained.

1. temperatureThe reaction mixture is heated under argon
2. temperatureat reflux for 16 h
3. temperatureIt is then cooled in order
4. customto be evaporated
5. customa rotary evaporator under reduced pressure (5 kPa)
6. addition200 cm3 of dichloromethane and 150 cm3 of water are added
7. extractionThe aqueous phase is extracted with 50 cm3 of dichloromethane
8. washwashed with 50 cm3 of a saturated aqueous solution of sodium chloride
9. dry with materialdried over sodium sulfate
10. concentrationconcentrated
11. customa rotary evaporator under reduced pressure (5 kPa)
12. customThe ochre product obtained
13. customis purified by flash chromatography over silica (column: 200 g; particle size: 15-40 μm; eluent: 100% dichloromethane)
14. concentrationAfter concentrating the fractions under reduced pressure, 2.09 g of 6-chloro-8-iodo-3-(1-propylbutyl)quinazolin-4(3H)-one
15. customare obtained