反应详情

温度

70 °C

105.6 g of finely pulverised potassium hydroxide are introduced into a solution of 92.9 g of N,N′-diacetylhydrazine and 1410 g of dimethyl sulfoxide. When the heat of reaction has died away, 229.9 g of 2,2′-dichlorodiethyl ether are added and then 221.1 g of finely ground potassium carbonate are introduced. The reaction mixture is heated to 70° C. and maintained at 70 to 75° C. for 2 hours, then cooled to 20 to 25° C. and filtered, and the filtration residue is washed with dimethyl sulfoxide. Concentration of the combined filtrates by evaporation yields an oil, to which 157 g of isopropanol are added. After cooling to −10° C., filtration is carried out and the crystalline residue is washed with isopropanol. After drying of the residue, 99.4 g (65.1%) of 4,5-diacetyl-[1,4,5]-oxadiazepine are obtained in a purity of 97.6%.

1. temperatureWhen the heat of reaction
2. temperaturemaintained at 70 to 75° C. for 2 hours
3. temperaturecooled to 20 to 25° C.
4. filtrationfiltered
5. washthe filtration residue is washed with dimethyl sulfoxide
6. customConcentration of the combined filtrates by evaporation
7. customyields an oil
8. temperatureAfter cooling to −10° C.
9. filtrationfiltration
10. washthe crystalline residue is washed with isopropanol
11. dry with materialAfter drying of the residue, 99.4 g (65.1%) of 4,5-diacetyl-[1,4,5]-oxadiazepine
12. customare obtained in a purity of 97.6%