Phosgene → 5-(1-Methylcyclopropyl)-1,3,4-oxadiazol-2(3H)-one
Reaktionsgleichung
[CH3:1][C:2]1([C:5]([NH:7][NH2:8])=[O:6])[CH2:4][CH2:3]1.[C:9](Cl)(Cl)=[O:10]>C(Cl)Cl>[O:10]=[C:9]1[O:6][C:5]([C:2]2([CH3:1])[CH2:4][CH2:3]2)=[N:7][NH:8]1Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
85 gm of 1-methylcyclopropane carboxylic acid hydrazide was added to methylene chloride on a 3-neck 2-liter round bottom flask. The system was first cooled to 0°-5° C. and 590.5 gm of a 12.5% solution of phosgene added dropwise over a period of time. The system was then heated at reflux for 7 hours. The methylene chloride was removed by stripping. The product was washed with petroleum ether and filtered to give 66.6 gm of 5-oxo-2-(1'-methylcyclopropyl)-1,3,4-oxadiazoline as light brown crystals, melting point 68°-70° C.
Aufarbeitung
- temperatureThe system was first cooled to 0°-5° C.
- temperatureThe system was then heated
- temperatureat reflux for 7 hours
- customThe methylene chloride was removed by stripping
- washThe product was washed with petroleum ether
- filtrationfiltered
Quellen und Nachweise
- ORD-Eintrag
- ord-de7d6322833c4040896f8278714e7f93
- Quelldatensatz
- uspto-grants-1986_04
- Patentnummer
- US04582828
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