反应详情

At a temperature and in the manner as indicated in Example 1, 39 g of potassium thiocyanate (0.4 mol) and 46 g of 4-methyl-thioanisol (0.33 mol) are stirred with 0.3 l of 98% hydrofluoric acid. The mixture is then stirred first for 10 hours at room temperature and then for 3 hours in a steel autoclave at 40° - 50° C, subsequently cooled, the reaction mixture is poured onto ice, the 4-methyl-thioanisol-2-thiocarboxylic acid amide precipitated is suction-filtered and dried. The yield (54 g) is 81% of the theoretical yield, relative to the 4-methyl-thioanisol used. After recrystallization of the product from chlorobenzene, the melting point is 160° C.

1. temperaturesubsequently cooled
2. additionthe reaction mixture is poured onto ice
3. customthe 4-methyl-thioanisol-2-thiocarboxylic acid amide precipitated
4. filtrationis suction-filtered
5. customdried
6. customThe yield (54 g)
7. customAfter recrystallization of the product from chlorobenzene