반응 #739083

반응 방정식

4-Chloro-2-fluoro-5-hydroxyphenylhydrazine

2-acetylcyclohexanone

acetic acid

→

2-(4-chloro-2-fluoro-5-hydroxyphenyl)-3-methyl-4,5,6,7-tetrahydro-2H-indazole

수율 88.1%

용매

xylene

반응 조건

후처리

1. 1
   온도under reflux for 5 hours
2. 2
   기타while removing water
3. 3
   온도After cooling
4. 4
   농축the mixture was concentrated
5. 5
   기타the residue was purified by silica gel column chromatography

실험 절차

4-Chloro-2-fluoro-5-hydroxyphenylhydrazine (0.5 g), 2-acetylcyclohexanone (0.4 g) and a catalytic amount of acetic acid were admixed with xylene (15 ml), and the resultant mixture was heated under reflux for 5 hours while removing water. After cooling, the mixture was concentrated, and the residue was purified by silica gel column chromatography to obtain 0.7 g of 2-(4-chloro-2-fluoro-5-hydroxyphenyl)-3-methyl-4,5,6,7-tetrahydro-2H-indazole. m.p., 188.5°-190° C.

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