反应详情

A 1-liter stirred autoclave was charged with 55.6 g (0.150 mole) of 1,2-diphenyl-4-p-t-butylphenylbutane-1,4-dione, 100 ml of xylene, 33.3 g (0.075 mole) of phosphorus pentasulfide and 130 g of hydrogen sulfide. The reactor was cooled and vented. The residue was stirred with 150 ml of absolute ethanol. Filtration gave a first crop of 18 g (32.6%) m.p. 108°-112° C. Chilling the filtrate and refiltering gave a second crop of 24 g (43.4%) m.p. 102°-105° C. The two crops were combined for recrystallization from a mixture of 50 ml of dioxane and 100 ml of absolute ehtanol. The pure product (31.3 g, 56.6%) had a m.p. of 117°-119° C.

1. temperatureThe reactor was cooled
2. filtrationFiltration
3. customgave a first crop of 18 g (32.6%) m.p. 108°-112° C
4. temperatureChilling the filtrate and refiltering
5. customgave a second crop of 24 g (43.4%) m.p. 102°-105° C
6. customThe two crops were combined for recrystallization from a mixture of 50 ml of dioxane and 100 ml of absolute ehtanol