反应详情

The title compound is prepared according to the procedure described by K. Takeda [J. Org. Chem., 50, 273, (1985)]. A mixture of 4-chloro-3-nitro-α,α,α-trifluorotoluene (50.0 g, 0.22 moles) and hydrazine hydrate (33.0, 0.33 moles) in absolute ethanol (75 ml) is refluxed for 24 h. After removal of the solvent under reduced pressure, the residue is dissolved in 10% aqueous sodium carbonate solution. The solution is washed with ether to remove the starting material and acidified with concentrated HCl to precipitate the product, which is washed with water and dried to obtain 40.0 g of the title compound. This product is recrystallized from ether.

1. customThe title compound is prepared
2. temperatureis refluxed for 24 h
3. customAfter removal of the solvent under reduced pressure
4. dissolutionthe residue is dissolved in 10% aqueous sodium carbonate solution
5. washThe solution is washed with ether
6. customto remove the starting material
7. customto precipitate the product, which
8. washis washed with water
9. customdried