Potassium Carbonate → 3-[7-[(3,5-dimethylisoxazol-4-yl)methyl]-5-methyl-2-(1-naphthylmethyl)-4,6-dioxo-4,5,6,7-tetrahydro-2H-pyrazolo[3,4-d]pyrimidin-3-yl]benzoic acid

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Reaktionsgleichung

Cl[CH2:2][C:3]1[C:4]([CH3:9])=[N:5][O:6][C:7]=1[CH3:8].[CH3:10][N:11]1[C:16](=[O:17])[C:15]2=[C:18]([C:32]3[CH:33]=[C:34]([CH:38]=[CH:39][CH:40]=3)[C:35]([OH:37])=[O:36])[N:19]([CH2:21][C:22]3[C:31]4[C:26](=[CH:27][CH:28]=[CH:29][CH:30]=4)[CH:25]=[CH:24][CH:23]=3)[N:20]=[C:14]2[NH:13][C:12]1=[O:41].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[CH3:9][C:4]1[C:3]([CH2:2][N:13]2[C:14]3=[N:20][N:19]([CH2:21][C:22]4[C:31]5[C:26](=[CH:27][CH:28]=[CH:29][CH:30]=5)[CH:25]=[CH:24][CH:23]=4)[C:18]([C:32]4[CH:33]=[C:34]([CH:38]=[CH:39][CH:40]=4)[C:35]([OH:37])=[O:36])=[C:15]3[C:16](=[O:17])[N:11]([CH3:10])[C:12]2=[O:41])=[C:7]([CH3:8])[O:6][N:5]=1

Komponenten

Reaktionsbedingungen

Temperatur: 85 °C

Versuchsvorschrift

4-(chloromethyl)-3,5-dimethylisoxazole (0.145 g) was added to a suspension of Resin bound 3-[5-methyl-2-(1-naphthylmethyl)-4,6-dioxo-4,5,6,7-tetrahydro-2H-pyrazolo[3,4-d]pyrimidin-3-yl]benzoic acid (0.120 g) and potassium carbonate (0.397 g) in dimethylformamide (1 ml). Reaction mixture was shaken at 85° C. for 20 hours. The resin was filtered and washed (3 times) DMF, H2O, DMF, CH2Cl2, MeOH, CH2Cl2, and dried in vacuum to give the subtitle compound.

Aufarbeitung

customReaction mixture
filtrationThe resin was filtered
washwashed (3 times) DMF, H2O, DMF, CH2Cl2, MeOH, CH2Cl2
customdried in vacuum

Quellen und Nachweise

ORD-Eintrag: ord-0c1d276037f241ebb8bac85f0f991fd6
Quelldatensatz: uspto-grants-2007_10
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US07285558B2

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