反应详情

In 40 ml of ethanol, 7.30 g (0.0244 mol) of the nitro compound obtained in Example 1 was dissolved. The solution was added with 0.1 g of 10% Pd-C and 3.66 g (0.073 mol) of hydrazine hydrate and refluxed on a hot water bath for one hour. After allowed to cool by itself, the solution was passed through a Celite layer to filter out the catalyst and then washed with ethanol. The filtrate was concentrated, dissolved in dichloromethane, washed with water, a saturated sodium bicarbonate aqueous solution and a saturated sodium chloride aqueous solution, and dried over anhydrous potassium carbonate. The solvents were distilled off and the residue was fractionally distilled, collecting the fraction having a boiling point of 82°-83° C. at 0.18 mmHg. There was obtained 6.09 g of 3-(2,2,3,3,3-pentafluoropropoxy)methyl-4-methylaniline in a 93% yield.

1. temperaturerefluxed on a hot water bath for one hour
2. temperatureto cool by itself
3. filtrationto filter out the catalyst
4. washwashed with ethanol
5. concentrationThe filtrate was concentrated
6. dissolutiondissolved in dichloromethane
7. washwashed with water
8. dry with materiala saturated sodium bicarbonate aqueous solution and a saturated sodium chloride aqueous solution, and dried over anhydrous potassium carbonate
9. distillationThe solvents were distilled off
10. distillationthe residue was fractionally distilled
11. customcollecting the fraction