反应详情

温度

-50 °C

8.3 ml of triethylamine are added dropwise to a suspension of 8.59 g of 5-oxo-2,2,4-trimethyl-3-thiazoline oxime in a solution of 10.0 g of bis-(N-methyl-N-fluorocarbonylamino)sulfide in 100 ml of absolute toluene, cooled to -50° C. The resulting clear solution is allowed to warm slowly to 0° C. during 11/2 hours, during which time a crystalline product is precipitated. The reaction mixture is poured into ice-cold brine and extracted with ethyl acetate. After drying the organic phase over anhydrous sodium sulfate and evaporating it, the resulting residue is purified by chromatography on silica gel (eluent:ethyl acetate/n-hexane 1:1). Crystallization from ethyl acetate/n-hexane yields 5-oxo-2,2,4-trimethyl-3-thiazoline O-[N-(N-methylfluoroformamidothio)-N-methylcarbamoyl]oxime, m.p. 77°-79° C.

1. temperatureto warm slowly to 0° C. during 11/2 hours
2. customduring which time a crystalline product is precipitated
3. additionThe reaction mixture is poured into ice-cold brine
4. extractionextracted with ethyl acetate
5. dry with materialAfter drying the organic phase over anhydrous sodium sulfate
6. customevaporating it
7. customthe resulting residue is purified by chromatography on silica gel (eluent:ethyl acetate/n-hexane 1:1)
8. customCrystallization from ethyl acetate/n-hexane