반응 #739081

반응 방정식

4-Chloro-2-fluoro-5-isopropoxyphenylhydrazine

2-acetylcyclohexanone

acetic acid

→

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

수율 39.1%

용매

xylene

반응 조건

후처리

1. 1
   온도under reflux for 8 hours
2. 2
   기타while removing water
3. 3
   온도After cooling
4. 4
   농축the reaction mixture was concentrated under reduced pressure
5. 5
   기타the residue was purified by silica gel column chromatography

실험 절차

4-Chloro-2-fluoro-5-isopropoxyphenylhydrazine (1.8 g), 2-acetylcyclohexanone (1.0 g) and a catalytic amount of acetic acid were dissolved in xylene (5 ml). The resultant mixture was heated under reflux for 8 hours while removing water. After cooling, the reaction mixture was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography to give 0.9 g of 3-methyl-2-(4-chloro-2-fluoro-5-isopropoxyphenyl)-4,5,6,7-tetrahydro-2H-indazole (Compound No. 5). nD14.5 1.5607.

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