反应详情

温度

100 °C

A mixture comprising 20 ml of ethylene glycol monomethyl ether and 70 mg of 55% sodium hydride was heated to 100° C., followed by the addition of a mixture comprising 500 mg of 2,6-dichloro-4-(3,4-methylenedioxybenzyl)aminoquinazoline and 5 ml of ethylene glycol monomethyl ether. The obtained mixture was heated under reflux for 2 hours and poured into 50 ml of water. The obtained mixture was extracted with 50 ml of ethyl acetate twice. The organic layers were together washed with 70 ml of an aqueous solution of sodium chloride twice, dried over magnesium sulfate and concentrated under a reduced pressure to give a crystalline residue. This residue was reprecipitated from ethyl acetate/n-hexane to give 420 mg of the title compound.

1. temperatureThe obtained mixture was heated
2. temperatureunder reflux for 2 hours
3. extractionThe obtained mixture was extracted with 50 ml of ethyl acetate twice
4. washThe organic layers were together washed with 70 ml of an aqueous solution of sodium chloride twice
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated under a reduced pressure
7. customto give a crystalline residue
8. customThis residue was reprecipitated from ethyl acetate/n-hexane