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Reaktionsgleichung

[NH:1]([C:8]1[N:13]=[C:12]2[N:14]([C:27]3[CH:32]=[CH:31][CH:30]=[C:29]([CH2:33][CH2:34]OS(C)(=O)=O)[CH:28]=3)[C:15](=[O:26])[N:16]([C:18]3[C:23]([CH3:24])=[CH:22][CH:21]=[CH:20][C:19]=3[Cl:25])[CH2:17][C:11]2=[CH:10][N:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:40]1(=[O:50])[NH:44][C:43](=[O:45])[C:42]2=[CH:46][CH:47]=[CH:48][CH:49]=[C:41]12.[K]>CN(C)C=O>[NH:1]([C:8]1[N:13]=[C:12]2[N:14]([C:27]3[CH:32]=[CH:31][CH:30]=[C:29]([CH2:33][CH2:34][N:44]4[C:40](=[O:50])[C:41]5=[CH:49][CH:48]=[CH:47][CH:46]=[C:42]5[C:43]4=[O:45])[CH:28]=3)[C:15](=[O:26])[N:16]([C:18]3[C:23]([CH3:24])=[CH:22][CH:21]=[CH:20][C:19]=3[Cl:25])[CH2:17][C:11]2=[CH:10][N:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Komponenten

Reaktionsbedingungen

Temperatur: 90 °C

Versuchsvorschrift

A solution of 233 mg (0.41 mmol) of 7-anilino-3-(2-chloro-6-methylphenyl)-3,4-dihydro-1-[3-(2-methanesulfonyloxyethyl)phenyl]pyrimido[4,5-d]pyrimidin-2(1H)-one in 10 ml of dimethylformamide was treated with 100 mg (0.54 mmol) of potassium phthalimide and the mixture heated at 90° C. for 3 hours. The mixture was cooled and evaporated. The residue was partitioned between 50 ml of ethyl acetate and 50 ml of water. The organic phase was dried over magnesium sulfate, filtered and evaporated to give 250 mg (99%) of 7-anilino-3-(2-chloro-6-methylphenyl)-3,4-dihydro-1-[3-(2-phthalimidoethyl)phenyl]-pyrimido[4,5-d]pyrimidin-2(1H)-one as a white solid. [Mass spectrum (ESI) MH+ =615].

Aufarbeitung

temperatureThe mixture was cooled
customevaporated
customThe residue was partitioned between 50 ml of ethyl acetate and 50 ml of water
dry with materialThe organic phase was dried over magnesium sulfate
filtrationfiltered
customevaporated

Quellen und Nachweise

ORD-Eintrag: ord-f771b07057db4de19b79032e42443ed0
Quelldatensatz: uspto-grants-2000_11
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US06150373

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