反应详情

The procedure is as Example 7, starting with 6-trifluoromethoxy-4-nitro-2-benzothiazolamine, iron powder, concentrated hydrochloric acid and ethanol having a water content of 50% (vol./vol.). After purification on a column of silica with a mixture of cyclohexane and ethyl acetate (10:90 by volume) as eluant, a white solid (1.5 g) is recovered, which solid is recrystallized in toluene (130 cc) to obtain 6-tri-fluoromethoxy-2,4-benzothiazolediamine (1 g), m.p. 206° C.

1. customAfter purification on a column of silica
2. additionwith a mixture of cyclohexane and ethyl acetate (10:90 by volume) as eluant
3. customa white solid (1.5 g) is recovered
4. customwhich solid is recrystallized in toluene (130 cc)