Reaktionsgleichung
NC1C=CN=C(C2C=CC=CN=2)N=1.C(OC=C(C(OCC)=O)C(OCC)=O)C.CS(O)(=O)=O.[N:34]1[CH:39]=[CH:38][CH:37]=[CH:36][C:35]=1[C:40]1[N:45]=[C:44]([NH:46][CH:47]=[C:48]([C:54]([O:56][CH2:57][CH3:58])=[O:55])[C:49]([O:51][CH2:52][CH3:53])=[O:50])[CH:43]=[CH:42][N:41]=1>>[N:34]1[CH:39]=[CH:38][CH:37]=[CH:36][C:35]=1[C:40]1[N:45]=[C:44]([NH:46][CH:47]=[C:48]([C:54]([O:56][CH2:57][CH3:58])=[O:55])[C:49]([O:51][CH2:52][CH3:53])=[O:50])[CH:43]=[CH:42][N:41]=1Komponenten
4
Versuchsvorschrift
A mixture containing 8.7 g. of 4-amino-2-(2-pyridinyl)pyrimidine and 14.2 g. of diethyl ethoxymethylenemalonate was heated in an oil bath at 130°-140° C. for one hour and then cooled to room temperature. To the cooled reaction mixture was added with stirring 300 ml. of ether and the mixture was filtered. To the filtrate was added 4.8 g. of methanesulfonic acid dissolved in 25 ml. of ethanol whereupon there separated an oily material which became a crystalline solid on standing. The solid was collected and recrystallized from ether-ethanol to yield 10.4 g. of diethyl N-[2-(2-pyridinyl)-4-pyrimidinyl]aminomethylenemalonate methanesulfonate, m.p. 162°-164° C.
Aufarbeitung
- additionA mixture containing 8.7 g
- customTo the cooled reaction mixture
- additionwas added
- filtrationof ether and the mixture was filtered
- additionTo the filtrate was added 4.8 g
- dissolutionof methanesulfonic acid dissolved in 25 ml
- customof ethanol whereupon there separated an oily material which
- customThe solid was collected
- customrecrystallized from ether-ethanol
- customto yield 10.4 g
Quellen und Nachweise
- ORD-Eintrag
- ord-ad6d4ba8d1404c4284d2c37bdce2a126
- Quelldatensatz
- uspto-grants-1977_06
- Patentnummer
- US04032523
Verknüpfte Notizen
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