反应详情

To a stirred mixture of 5 g (0.035 mole) 2-(1'-methylcyclopropyl)-5-oxo-1,3,4-oxadiazoline and 13.5 g (0.035 mole) triphenyl tin chloride in methylene chloride (about 100 ml), 3.5 g (0.035 mole) triethylamine in methylene chloride (about 50 ml) was added dropwise. The reaction mixture was allowed to stir overnight at ambient temperature. The reaction mixture was refluxed (at about 40° C.) for about 3 hours, cooled and then allowed to stir at ambient temperature for about one hour. The reaction mixture was washed with water and then extracted with methylene chloride. The methylene chloride extract was dried and then stripped. The residue was washed with hexane to precipitate the above-identified product, melting point 165°-167° C.

1. additionwas added dropwise
2. temperatureThe reaction mixture was refluxed (at about 40° C.) for about 3 hours
3. temperaturecooled
4. stirringto stir at ambient temperature for about one hour
5. washThe reaction mixture was washed with water
6. extractionextracted with methylene chloride
7. extractionThe methylene chloride extract
8. customwas dried
9. washThe residue was washed with hexane
10. customto precipitate the above-identified product, melting point 165°-167° C.