Reaktionsgleichung
C1(N[C:7]2[C:12]([CH3:13])=[C:11]([CH3:14])[N:10]=[C:9]([NH:15][CH2:16][C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][N:18]=3)[N:8]=2)CCCC1.[CH3:23][CH:24]1[CH2:29][CH2:28][CH2:27][CH2:26][CH:25]1[NH2:30]>>[CH3:13][C:12]1[C:7]([NH:30][CH:25]2[CH2:26][CH2:27][CH2:28][CH2:29][CH:24]2[CH3:23])=[N:8][C:9]([NH:15][CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][N:18]=2)=[N:10][C:11]=1[CH3:14]Komponenten
Versuchsvorschrift
The titled compound was synthesized according to the procedure described for preparation of N4-cyclopentyl-5,6-dimethyl-N2-(pyridin-2-ylmethyl)pyrimidine-2,4-diamine (Example 29) using 2-methylcyclohexanamine instead of cyclopentanamine. The crude material was purified by column chromatography eluting with mixture of chloroform/ethanol/20% water solution of ammonia (200:10:1), and then the final product was washed with diethyl ether to afford the titled compound as a white solid. 1H NMR (400 MHz, CDCl3) δ ppm 0.93 (bs, 3H), 1.28-1.42 (m, 6H), 1.62-1.70 (m, 1H), 1.78-1.89 (m, 2H), 1.93 (s, 3H), 2.07 (s, 3H), 2.95-3.04 (m, 1H), 4.43 (bs, 2H), 7.22 (t, J=7.30 Hz, 1H), 7.56 (d, J=7.76 Hz, 1H), 7.68-7.75 (m, 1H), 8.65 (d, J=4.92 Hz, 1H); MS (ESI) m/z 326.4.0 (M+1)+.
Aufarbeitung
- customThe titled compound was synthesized
- customThe crude material was purified by column chromatography
- washeluting with mixture of chloroform/ethanol/20% water solution of ammonia (200:10:1)
- washthe final product was washed with diethyl ether
Quellen und Nachweise
- ORD-Eintrag
- ord-b893dc03463344a1bf88d4a04a2f5e15
- Quelldatensatz
- uspto-grants-2016_09
- Patentnummer
- US09447051B2
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