反应详情

温度

120 °C

) 3.3 g (30 mmol) of aminomethanephosphonic acid is introduced into 120 ml of water and 120 ml of acetonitrile together with 3.37 g (31.8 mmol) of soda and mixed with 7.8 g (97%, 30 mmol) of 3-trifluoromethyl-4,6-dichloronitrobenzene and refluxed for 4 hours at a bath temperature of 120° C. After the acetonitrile is drawn off in a rotary evaporator, it is extracted three times with 100 ml of ethyl acetate. The organic phase is washed with a little water. It contains starting material and is discarded. The collected aqueous phase is made acidic at pH 1 with 4N hydrochloric acid and extracted three times with 100 ml of ethyl acetate each. The organic phase is washed with water, dried, filtered and concentrated by evaporation. 6.85 g (68% of theory) of N-(2-nitro-4-trifluoromethyl-5-chloro-phenyl)-aminomethanephosphonic acid with a melting point of 207.3° C. is obtained.

1. customAfter the acetonitrile is drawn off in a rotary evaporator, it
2. extractionis extracted three times with 100 ml of ethyl acetate
3. washThe organic phase is washed with a little water
4. extractionextracted three times with 100 ml of ethyl acetate each
5. washThe organic phase is washed with water
6. customdried
7. filtrationfiltered
8. concentrationconcentrated by evaporation