Hydrochloric Acid → HCID 20535105, Verbindung
Reaktionsgleichung
[NH2:1][C:2]1[N:7]2[O:8][C:9](=[O:11])[N:10]=[C:6]2[N:5]=[C:4]([N:12]([CH2:16][CH:17]=[CH2:18])[CH2:13][CH:14]=[CH2:15])[N:3]=1.[CH3:19][O:20][CH2:21][C:22](Cl)=[O:23].Cl>O.C(Cl)Cl.C(N(CC)CC)C>[CH2:13]([N:12]([CH2:16][CH:17]=[CH2:18])[C:4]1[N:3]=[C:2]([NH:1][C:22](=[O:23])[CH2:21][O:20][CH3:19])[N:7]2[O:8][C:9](=[O:11])[N:10]=[C:6]2[N:5]=1)[CH:14]=[CH2:15]Komponenten
Reaktionsbedingungen
- Temperatur
- 5 °C
Versuchsvorschrift
5.0 g. of 7-amino-5-diallylamino-2H-[1,2,4]oxadiazolo[2,3-a]-s-triazin-2-one are suspended in 100 ml. of methylene chloride and 10 ml. of triethylamine. 2.5 g. of methoxyacetyl chloride in 20 ml. of methylene chloride are added dropwise while stirring and cooling to about 5° C. After 1 hour at about 5° C., the mixture is treated with water and adjusted to pH 4 with 3-N hydrochloric acid. The two phases are separated and the aqueous phase is extracted with methylene chloride. The combined organic extracts are dried over sodium sulfate and evaporated under reduced pressure. The residue is recrystallized from methylene chloride and diethyl ether, there being obtained N-{5-diallylamino-2-oxo-2H-[1,2,4]oxadiazolo[2,3-a]-s-triazin-7-yl}-2-methoxyacetamide having a melting point of 135°-136° C.
Aufarbeitung
- customThe two phases are separated
- extractionthe aqueous phase is extracted with methylene chloride
- dry with materialThe combined organic extracts are dried over sodium sulfate
- customevaporated under reduced pressure
- customThe residue is recrystallized from methylene chloride and diethyl ether, there
Quellen und Nachweise
- ORD-Eintrag
- ord-504e016bb80347938b8c00fc743cfeda
- Quelldatensatz
- uspto-grants-1981_06
- Patentnummer
- US04276417
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