反应详情

In 40 ml of acetic acid was dissolved 3.0 g of 3,5-dichloro-4-(3,4-dichloro-α-cyanobenzyl)aniline. To the solution was then added 3 ml of 35% hydrochloric acid. To the mixture was added dropwise, while cooling at temperatures ranging from 10 to 12° C., a solution of 0.8 g of 98.5% sodium nitrite in 3 ml of water. The reaction mixture was stirred for 40 minutes under the same conditions, to which was then added 7.0 g of stannous chloride dissolved in 10 ml of 35% hydrochloric acid. The reaction mixture was poured into ice-water, which was then made into alkaline, followed by extraction with 200 ml of ethyl acetate. The extract was washed with water, dried over anhydrous magnesium sulfate, and concentrated to afford the titled compound in a yield of 96%, m.p.183-185° C.

1. additionTo the mixture was added dropwise
2. temperaturewhile cooling at temperatures
3. customranging from 10 to 12° C.
4. extractionfollowed by extraction with 200 ml of ethyl acetate
5. washThe extract was washed with water
6. dry with materialdried over anhydrous magnesium sulfate
7. concentrationconcentrated