反应详情

A 1-liter stainless steel stirred autoclave was charged with 33 g. (0.0946 mole) of 1,2-diphenyl-4-o-chlorophenylbutane-1,4-dione, 100 ml. of xylene, 20 g of phosphorus pentasulfide and 125 g of hydrogen sulfide. The autoclave was then heated at 160°-187° C. for three hours. The autoclave was cooled and vented. The residue was washed with ethanol and filtered off to give 17 g (51.8%) of crude product, m.p. 103°-107° C. Recrystallization from 20 ml of dioxane and 40 ml of ethanol gave 10.5 g (32%) of pure product, m.p. 117°-118° C.

1. temperatureThe autoclave was then heated at 160°-187° C. for three hours
2. temperatureThe autoclave was cooled
3. washThe residue was washed with ethanol
4. filtrationfiltered off
5. customto give 17 g (51.8%) of crude product, m.p. 103°-107° C
6. customRecrystallization from 20 ml of dioxane and 40 ml of ethanol