Reaktionsgleichung
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[CH2:7][NH:8][C:9](=[O:31])[C:10]1[CH:15]=[CH:14][C:13]([O:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH3:30])=[CH:12][CH:11]=1.[CH3:32][I:33]>>[I-:33].[CH3:32][N+:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[CH2:7][NH:8][C:9](=[O:31])[C:10]1[CH:11]=[CH:12][C:13]([O:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH3:30])=[CH:14][CH:15]=1Komponenten
3
Versuchsvorschrift
A mixture of 1.0 g of product from Example 4 and 7.33 ml of methyl iodide is heated, in a dark sealed tube, at 100°-120° C. for 22 hours. The cooled reaction mixture is concentrated in vacuo and recrystallized 2 times from methyl alcohol to give 1.15 g of the desired product as light yellow microneedles.
Aufarbeitung
- temperatureis heated, in a dark sealed tube, at 100°-120° C. for 22 hours
- customThe cooled reaction mixture
- concentrationis concentrated in vacuo
- customrecrystallized 2 times from methyl alcohol
Quellen und Nachweise
- ORD-Eintrag
- ord-11dd4be9d0de4e58bbf14c8c3fe5d2bb
- Quelldatensatz
- uspto-grants-1993_05
- Patentnummer
- US05208247
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