Reaktionsgleichung
C(O[CH2:4][CH2:5][C:6]#[N:7])C.C(O)C.[NH:11]([C:13]1[S:14][C:15]2[CH:21]=[CH:20][CH:19]=[CH:18][C:16]=2[N:17]=1)[NH2:12].OCC[N+](C)(C)C>CO>[NH2:7][C:6]1[CH2:5][CH2:4][N:11]([C:13]2[S:14][C:15]3[CH:21]=[CH:20][CH:19]=[CH:18][C:16]=3[N:17]=2)[N:12]=1Komponenten
6
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
A mixture of 5.0 g. of β-ethoxypropionitrile, 100 ml. of absolute ethanol, 8.25 g. of 2-hydrazinobenzothiazole and 2.5 g. of 50% w/v choline in methanol is refluxed on a steam bath for 16 hours, then the solvent is removed in vacuo. Water is added and the solid is collected by filtration. The solid is recrystalized twice from ethanol to give 5.75 g. of the product of the Example as grey prisms, m.p. 231.5°-235° C.
Aufarbeitung
- additionA mixture of 5.0 g
- temperatureis refluxed on a steam bath for 16 hours
- customthe solvent is removed in vacuo
- additionWater is added
- filtrationthe solid is collected by filtration
- customThe solid is recrystalized twice from ethanol
- customto give 5.75 g
Quellen und Nachweise
- ORD-Eintrag
- ord-96eb4ec0f63c4844ba66b37c8d009237
- Quelldatensatz
- uspto-grants-1986_11
- Patentnummer
- US04622401
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