تفاعل #2252952

معادلة التفاعل

1,2,4-triazole sodium salt

potassium iodide

2-(2'-difluoromethoxy-4'-chlorophenyl)-2-bromomethyl-4-ethyl-1,3-dioxolane

water

→

2-[2'-Difluoromethoxy-4'-chlorophenyl]-2-(1H-1,2,4-triazolylmethyl)-4-ethyl-1,3-dioxolane

المذيبات

dimethylformamide

ظروف التفاعل

المعالجة

1. 1
   استخلاصextracted with 2×300 ml of diethyl ether
2. 2
   غسيلThe combined organic phases are washed with 2×200 ml of water
3. 3
   تجفيفdried over sodium sulfate
4. 4
   ترشيحfiltered
5. 5
   أخرىthe solvent is removed by evaporation
6. 6
   أخرىThe oily residue is chromatographed through a 50 cm column of silica gel with a 1:1 mixture of methylene chloride/diethyl ether as eluant
7. 7
   أخرىThe eluant is removed by evaporation
8. 8
   أخرىto give a yellow oil with a refractive index nD27

الإجراء التجريبي

5.9 parts of 1,2,4-triazole sodium salt, a catalytic amount of potassium iodide and 12 parts of the 2-(2'-difluoromethoxy-4'-chlorophenyl)-2-bromomethyl-4-ethyl-1,3-dioxolane prepared in (b) are stirred in 100 ml of dimethylformamide for 16 hours at a bath temperature of 130° C. The reaction mixture is cooled to room temperature, poured into 500 ml of water and extracted with 2×300 ml of diethyl ether. The combined organic phases are washed with 2×200 ml of water, dried over sodium sulfate, filtered, and the solvent is removed by evaporation. The oily residue is chromatographed through a 50 cm column of silica gel with a 1:1 mixture of methylene chloride/diethyl ether as eluant. The eluant is removed by evaporation to give a yellow oil with a refractive index nD27 : 1.5132.

المصدر