反应详情

A mixture of 12.90 g (0.025 mole) of 1-[2-(o-chlorobenzoyl)-4-chlorophenyl]-5-(iodomethyl)-1H-1,2,4-triazole-3-carboxylic acid methyl ester [see Example 13 (b)] and 11 ml of 33% ethanolic dimethylamine solution in 250 ml of methanol is stirred for 7 hours at room temperature. The reaction solution is thereupon concentrated in vacuo; water is added to the residue and the whole is extracted twice with methylene chloride. The organic phase is washed twice with water and once with saturated sodium chloride solution; it is dried over sodium sulphate and concentrated in vacuo to dryness. The amorphous residue is dissolved in 130 ml of ether; the solution is allowed to stand and the reaction product then crystallises out. It is filtered off with suction and washed with ether. After drying there is obtained 1-[2-(o-chlorobenzoyl)-4-chlorophenyl)-5-[(dimethylamino)-methyl]-1H-1,2,4-triazole-3-carboxylic acid methyl ester, m.p. 131°-134°.

1. concentrationThe reaction solution is thereupon concentrated in vacuo
2. additionwater is added to the residue
3. extractionthe whole is extracted twice with methylene chloride
4. washThe organic phase is washed twice with water and once with saturated sodium chloride solution
5. dry with materialit is dried over sodium sulphate
6. concentrationconcentrated in vacuo to dryness
7. dissolutionThe amorphous residue is dissolved in 130 ml of ether
8. customthe reaction product then crystallises out
9. filtrationIt is filtered off with suction
10. washwashed with ether
11. customAfter drying there