反应详情

10 g (0.0628 mol) of 2,4-difluoronitrobenzene was stirred for 4 days with 4.36 g (0.0728 mol) of N,N-dimethylhydrazine in 7.08 g of triethylamine and 100 ml methanol. The mixture was concentrated and the resulting solid dissolved in methylene chloride, washed with water and brine, dried with MgSO4 and concentrated to yield an orange solid. The solid was triturated in 95% ethanol/water, filtered and dried to give 6.1 g 4-fluoro-2-(2,2-dimethylhydrazino) nitrobenzene, m.p. 67°-71° C.

1. concentrationThe mixture was concentrated
2. dissolutionthe resulting solid dissolved in methylene chloride
3. washwashed with water and brine
4. dry with materialdried with MgSO4
5. concentrationconcentrated
6. customto yield an orange solid
7. customThe solid was triturated in 95% ethanol/water
8. filtrationfiltered
9. customdried