反应详情

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 2-oxo-5-(1'-methylcyclopropyl)-1,3,4-oxadiazoline as light brown crystals, m.p. 68°-70° C.

1. temperatureThe system was first cooled to 0°-5° C.
2. temperatureThe system was then heated
3. temperatureat reflux for 7 hours
4. customThe methylene chloride was removed by stripping
5. washThe product was washed with petroleum ether
6. filtrationfiltered