反应详情

A solution of 106.2 g (0.250 mole) of 1-[2-(o-chlorobenzoyl)-4-chlorophenyl]-5-(chloromethyl)-1H-1,2,4-triazole-3-carboxylic acid methyl ester and 56.2 g (0.375 mole) of sodium iodide in 2200 ml of acetone is refluxed for 40 minutes. The reaction mixture is thereupon concentrated in vacuo. Water is added to the residue, and extraction is performed twice with methylene chloride. The organic phase is washed twice with diluted aqueous sodium bisulphite solution and twice with saturated sodium chloride solution; it is dried over sodium sulphate and concentrated in vacuo. The residue is dissolved in the minimum amount of methylene chloride, and 400 ml of ether is slowly added with stirring, whereupon the reaction product crystallises out. After filtration with suction and drying in vacuum, there is obtained 1-[2-(o-chlorobenzoyl)-4-chlorophenyl]-5-(iodomethyl)-1H-1,2,4-triazole-3-carboxylic acid methyl ester, m.p. 125°-128°.

1. concentrationThe reaction mixture is thereupon concentrated in vacuo
2. additionWater is added to the residue, and extraction
3. washThe organic phase is washed twice with diluted aqueous sodium bisulphite solution and twice with saturated sodium chloride solution
4. dry with materialit is dried over sodium sulphate
5. concentrationconcentrated in vacuo
6. dissolutionThe residue is dissolved in the minimum amount of methylene chloride, and 400 ml of ether
7. additionis slowly added
8. customcrystallises out
9. filtrationAfter filtration with suction
10. customdrying in vacuum