Reaktionsgleichung
[NH2:1][C:2]1[N:7]=[C:6]([CH2:8][C:9]2[C:14]([Cl:15])=[CH:13][CH:12]=[CH:11][C:10]=2[Cl:16])[N:5]=[C:4]([NH:17][C:18]2[CH:25]=[CH:24][C:21]([C:22]#[N:23])=[CH:20][CH:19]=2)[N:3]=1.CO[CH:28](OC)[N:29]([CH3:31])[CH3:30]>>[Cl:16][C:10]1[CH:11]=[CH:12][CH:13]=[C:14]([Cl:15])[C:9]=1[CH2:8][C:6]1[N:7]=[C:2]([N:1]=[CH:28][N:29]([CH3:31])[CH3:30])[N:3]=[C:4]([NH:17][C:18]2[CH:19]=[CH:20][C:21]([C:22]#[N:23])=[CH:24][CH:25]=2)[N:5]=1Komponenten
3
Versuchsvorschrift
Compound (1) (0.0016 mol) and 1,1-dimethoxy-N,N-dimethylmethanamine (21 ml) were combined and stirred vigorously at ambient temperature for 8 hours. The reaction mixture was filtered and the collected solid was washed with ether (Fraction A). Additional compound was obtained by concentration of the filtrate (Fraction B). Fractions A and B were combined and recrystallized from ethanol, yielding 0.15 g of 4-[[4-[(2,6-dichlorophenyl)methyl]-6-[[(dimethylamino)methylene]amino]-1,3,5-triazin-2-yl]amino]benzonitrile (compound 62).
Aufarbeitung
- filtrationThe reaction mixture was filtered
- washthe collected solid was washed with ether (Fraction A)
- customAdditional compound was obtained by concentration of the filtrate (Fraction B)
- customrecrystallized from ethanol
Quellen und Nachweise
- ORD-Eintrag
- ord-039fc777b0a64bfcba2822c0ace28a59
- Quelldatensatz
- uspto-grants-2005_02
- Patentnummer
- US06858609B2
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