Cyclohexylamine → N-Cyclohexyl-4-fluoro-6-methoxy-2-pyrimidinamine
Reaktionsgleichung
[CH:1]1([NH2:7])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.F[C:9]1[N:14]=[C:13]([F:15])[CH:12]=[C:11]([O:16][CH3:17])[N:10]=1.C(OCCCC)CCC>>[CH:1]1([NH:7][C:9]2[N:14]=[C:13]([F:15])[CH:12]=[C:11]([O:16][CH3:17])[N:10]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1Komponenten
4
Versuchsvorschrift
10.1 g (0.102 mol) of cyclohexylamine were added at 0°-to 2° C. to a mixture of 7.3 g (0.05 mol) of 2,4-difluoro-6-methoxypyrimidine in 50 ml of methyl t.-butyl ether within 15 minutes. After 1 hour at 0° C. and 3 hours at 25° C., the resulting precipitate was filtered off, and the filtrate was washed with water, dried over magnesium sulfate and concentrated. 8.3 g (73.8% of theory) of the title compound were isolated as an oil (nD23 =1.5211) after chromatography of the residue obtained in this way.
Aufarbeitung
- filtration3 hours at 25° C., the resulting precipitate was filtered off
- washthe filtrate was washed with water
- dry with materialdried over magnesium sulfate
- concentrationconcentrated
Quellen und Nachweise
- ORD-Eintrag
- ord-1b876647b00948b9a608b102721ab20b
- Quelldatensatz
- uspto-grants-1991_04
- Patentnummer
- US05011927
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