反应详情

温度

180 °C

A mixture of 250 mg (0.67 mmol) of 3-(2,6-dichlorophenyl)-7-methanesulfonyl-3,4-dihydropyrimido[4,5-d]pyrimidin-2(1H)-one and 600 mg (2.9 mmol) of 4-[2-(diethylamino)ethoxy]aniline was heated at 180° C. for 35 minutes and then cooled. The residue was subjected to column chromatography on silica gel using dichloromethane/methanol/acetic acid/water 240:24:3:2 for the elution. Product-containing fractions were combined and evaporated and the residue was evaporated with toluene. The residue was dissolved in 30 ml of dichloromethane, washed twice with 20 ml of saturated aqueous sodium bicarbonate solution each time, dried over magnesium sulfate, filtered and evaporated. The residue was triturated in hexane, filtered off and dried to give 70 mg (21%) of 3-(2,6-dichlorophenyl)-7-[4-[2-(diethylamino)ethoxy]anilino]-3,4-dihydropyrimido[4,5-d]pyrimidin-2(1H)-one as an off-white solid of melting point 248° C.

1. temperaturecooled
2. washfor the elution
3. customevaporated
4. customthe residue was evaporated with toluene
5. dissolutionThe residue was dissolved in 30 ml of dichloromethane
6. washwashed twice with 20 ml of saturated aqueous sodium bicarbonate solution each time
7. dry with materialdried over magnesium sulfate
8. filtrationfiltered
9. customevaporated
10. customThe residue was triturated in hexane
11. filtrationfiltered off
12. customdried