반응 #80519

반응 방정식

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

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

o-dichlorobenzene

→

desired compound

수율 48.7%

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

수율 48.7%

용매

chloroform

반응 조건

후처리

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

실험 절차

A mixture of N-methyl-N-(p-toluenesulfonyl)-2-chloro-6-fluorobenzohydrazonoyl chloride (0.90 g), 4-(3-chloro-5-trifluoromethylpyridine-2-yloxy)-3methoxybenzonitrile (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 0.60 g of desired compound.

출처