反应详情

温度

0 °C

2',4'-Difluoro-2-(1H-1,2,4-triazol-1-yl)acetophenone hydrochloride (59.6 g, 0.23M), trimethylsulphoxonium iodide (50.6 g, 0.23M) and cetrimide (2.1 g) were stirred in a mixture of toluene (370 ml) and 20% w/w aqueous sodium hydroxide at 60° for 3 hours. The toluene layer was separated and concentrated to 110 ml then diluted with ethyl acetate (150 ml). A solution of methanesulphonic acid (16.6 g, 0.172M) in ethyl acetate (20 ml) was added. More ethyl acetate (100 ml) was added and the mixture was stirred at 0° C. for one hour then filtration of the precipitate gave the title compound (43 g, 56%).

1. customThe toluene layer was separated
2. concentrationconcentrated to 110 ml
3. additionthen diluted with ethyl acetate (150 ml)
4. additionA solution of methanesulphonic acid (16.6 g, 0.172M) in ethyl acetate (20 ml) was added
5. additionMore ethyl acetate (100 ml) was added
6. filtrationfiltration of the precipitate