تفاعل #80508

معادلة التفاعل

N-methyl-N-(p-toluenesulfonyl)-2-chloro-6-fluorobenzohydrazonoyl chloride

4-chloro-3-(5-trifluoromethylpyridine-2-yloxy)benzonitrile

o-dichlorobenzene

→

desired compound

المردود 31.1%

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

المردود 31.1%

المذيبات

chloroform

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

A mixture of N-methyl-N-(p-toluenesulfonyl)-2-chloro-6-fluorobenzohydrazonoyl chloride (1.00 g), 4-chloro-3-(5-trifluoromethylpyridine-2-yloxy)benzonitrile (0.90 g), anhydrous iron (III) chloride (0.50 g) and o-dichlorobenzene (5 ml) is stirred at an oil bath temperature of 140° C. for 30 minutes. After cooling, it is dissolved in chloroform (100 ml) and washed with dilute hydrochloric acid, dilute aqueous solution of sodium hydroxide and saline. Then, it is 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 0.40 g of desired compound.

المصدر