Reaktionsgleichung
[NH2:1][C:2]1[N:3]=[CH:4][C:5]2[CH:11]=[C:10]([C:12]3[C:17]([Cl:18])=[CH:16][CH:15]=[CH:14][C:13]=3[Cl:19])[C:9]([NH2:20])=[N:8][C:6]=2[N:7]=1.S(=O)(=O)(O)[NH2:22].[CH2:26]([N:28]([CH2:31][CH2:32]N)[CH2:29][CH3:30])[CH3:27]>>[Cl:19][C:13]1[CH:14]=[CH:15][CH:16]=[C:17]([Cl:18])[C:12]=1[C:10]1[C:9]([NH2:20])=[N:8][C:6]2[N:7]=[C:2]([NH:1][CH2:27][CH2:26][N:28]([CH2:31][CH3:32])[CH2:29][CH3:30])[N:3]=[CH:4][C:5]=2[CH:11]=1.[NH3:22]Komponenten
Reaktionsbedingungen
- Temperatur
- 150 °C
Versuchsvorschrift
A mixture of 2,7-diamino-6-(2,6-dichlorophenyl)-pyrido[2,3-d]pyrimidine (4.0 g) from Example 1, sulfamic acid (2.53 g), and diethylaminoethylamine (40 mL) was heated to approximately 150° C. for 20 hours. The excess diethylaminoethylamine was removed in vacuo. The resulting oil was dissolved in diethyl ether, diluted with hexane, and then filtered. The resulting solid was dissolved in dichloromethane which was washed several times with water, dried with magnesium sulfate, and concentrated in vacuo. The residue was crystallized from ethyl acetate to give the title compound 6-(2, 6-dichlorophenyl)-N2 -(2-diethylaminoethyl)-pyrido[2,3-d]pyrimidine-2,7-diamine, CIMS (1% NH3 in CH4): 433=M+ +C2H5, 405=M+ +H, 389=M+ -Et, 360; mp 216-219.5° C.
Aufarbeitung
- customThe excess diethylaminoethylamine was removed in vacuo
- dissolutionThe resulting oil was dissolved in diethyl ether
- additiondiluted with hexane
- filtrationfiltered
- dissolutionThe resulting solid was dissolved in dichloromethane which
- washwas washed several times with water
- dry with materialdried with magnesium sulfate
- concentrationconcentrated in vacuo
- customThe residue was crystallized from ethyl acetate
Quellen und Nachweise
- ORD-Eintrag
- ord-bdfaf0439762485e8efdeb2b7fae8ee4
- Quelldatensatz
- uspto-grants-1999_09
- Patentnummer
- US05952342
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