反应详情

310 ml (0.226 mole) of a 33% ethanolic dimethylamine solution is added to a suspension of 45.0 g (0.11 mole) of 1-[2-(o-chlorobenzoyl)-4-chlorophenyl]-5-(chloromethyl)-1H-1,2,4-triazole-3-carboxylic acid (see DT-OS 2,159,527, page 32) and 0.5 g (0.0033 mole) of sodium iodide in 250 ml of methanol, and the mixture is stirred for 6 hours at room temperature. The clear reaction solution is concentrated in vacuo; the residue is dissolved in 200 ml of water, and 2 N hydrochloric acid solution is slowly added until the pH value of 5 is reached. After 16 hours' standing at 0°-5°, the precipitated aminic acid is filtered off and well washed with water and then with ether. Upon drying, there is obtained 1-[2-(o-chlorobenzoyl)-4-chlorophenyl]-5-[(dimethylamino)-methyl]-1H-1,2,4-triazole-3-carboxylic acid, m.p. 222°-225° with decomposition.

1. concentrationThe clear reaction solution is concentrated in vacuo
2. dissolutionthe residue is dissolved in 200 ml of water
3. addition2 N hydrochloric acid solution is slowly added until the pH value of 5
4. waitAfter 16 hours' standing at 0°-5°
5. filtrationthe precipitated aminic acid is filtered off
6. washwell washed with water
7. customUpon drying