反应详情

In a 1-liter autoclave were place 30 g (82.8 mmoles) of 1,2-diphenyl-4-(3-fluoro-4-methoxyphenyl)butane-1,4-dione, 100 ml of xylene, 18.4 g (41.4 mmoles) of phosphorus pentasulfide and 130 g of hydrogen sulfide. The vessel was heated 205 minutes at 155°-163` C. (1145-1235 psig.). The reactor was cooled and the hydrogen sulfide vented into a solution of 200 g of sodium hydroxide in 2 l of water. The semisolid residue was stirred with 150 ml of absolute ethanol. Filtration gave a first crop of 14.7 g (49.3%) m.p. 122°-125° C. Chilling the filtrate and refiltration gave a second crop of 10.5 g (35.2%), m.p. 118°-122° C. The two crops were combined and recrystallized from a mixture of 30 ml of dioxane and 70 ml of absolute ethanol to give 21.5 g (72.0%) of colorless plates, m.p. 123°-125° C.

1. temperatureThe vessel was heated 205 minutes at 155°-163` C
2. temperatureThe reactor was cooled
3. filtrationFiltration
4. customgave a first crop of 14.7 g (49.3%) m.p. 122°-125° C
5. temperatureChilling the filtrate and refiltration
6. customgave a second crop of 10.5 g (35.2%), m.p. 118°-122° C
7. customrecrystallized from a mixture of 30 ml of dioxane and 70 ml of absolute ethanol
8. customto give 21.5 g (72.0%) of colorless plates, m.p. 123°-125° C.