Tetrabutylammonium Fluoride → Pyrimido[4,5-d]pyrimidin-2(1H)-one
反応式
[Si](OCCC1C=C([N:27]2[C:32]3=[N:33][C:34](NC4C=CC(OCCN(CC)CC)=CC=4)=[N:35][CH:36]=[C:31]3[CH2:30][N:29](C3C=CC(Cl)=CC=3Cl)[C:28]2=[O:60])C=CC=1)(C(C)(C)C)(C1C=CC=CC=1)C1C=CC=CC=1.[F-].C([N+](CCCC)(CCCC)CCCC)CCC>O1CCCC1>[NH:27]1[C:32]2=[N:33][CH:34]=[N:35][CH:36]=[C:31]2[CH:30]=[N:29][C:28]1=[O:60]参加物
4
実験手順
A solution of 200 mg (0.23 mmol) of 1-[3-(tert-butyldiphenylsilyloxyethyl)phenyl]-3-(2,4-dichlorophenyl)-7-[4-[2-(diethylamino)ethoxy]anilino]-3,4-dihydropyrimido[4,5-d]pyrimidin-2(1H)-one in 5 ml of tetrahydrofuran was treated with 0.5 ml (0.5 mmol) of a 1M solution of tetrabutylammonium fluoride in tetrahydrofuran. After 1 hour the mixture was evaporated and the product purified by chromatography on silica gel using dichloromethane/methanol in a ratio 20:1 as eluting solvent. Evaporation of the product-containing fractions followed by trituration of the residue with hexane and filtration gave 60 mg (42%) 3-(2,4-dichlorophenyl)-7-[4-[2-(diethylamino)ethoxy]anilino]-3,4-dihydro-1-[3-(2-hydroxyethyl))phenyl]pyrimido[4,5-d]pyrimidin-2(1H)-one as a white solid of melting point 110° C.