تفاعل #80495

معادلة التفاعل

chloroform

N-methyl-N-(methanesulfonyl)-2-chloro-6-fluorobenzohydrazonoyl chloride

4-(4-trifluoromethoxyphenyl)benzonitrile

chlorobenzene

→

desired compound

3-(2-chloro-6-fluorophenyl)-5-[2-chloro-4-(4-trifluoromethoxyphenyl)phenyl]1-methyl-1H-1,2,4-triazole

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةAfter cooling
2. 2
   غسيلwashed
3. 3
   workup.ADDITIONwith dilute hydrochrolic acid, dilute aqueous solution of sodium hydroxide and saline in this order
4. 4
   تجفيفdried over anhydrous magnesium sulfate
5. 5
   تركيزconcentrated under reduced pressure
6. 6
   أخرىThe concentrate is purified by silica gel column chromatography
7. 7
   workup.ADDITIONusing mixed solvent of hexane-ethyl acetate as eluent

الإجراء التجريبي

A mixture of N-methyl-N-(methanesulfonyl)-2-chloro-6-fluorobenzohydrazonoyl chloride (1.50 g), 4-(4-trifluoromethoxyphenyl)benzonitrile (1.56 g), anhydrous iron (III) chloride (0.90 g) and chlorobenzene (20 ml) is stirred at an oil bath temperature of 140° C. for 1 hour. After cooling, the reaction mixture is dissolved in chloroform (300 ml), washed with dilute hydrochrolic acid, dilute aqueous solution of sodium hydroxide and saline in this order, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The concentrate is purified by silica gel column chromatography using mixed solvent of hexane-ethyl acetate as eluent to give 1.80 g of desired compound (refractive index: 1.5925).

المصدر