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Ethyl 2-oxocyclohexanecarboxylate → 2-(4-Chloro-2-fluoro-5-hydroxyphenyl)-2,3a,4,5,6,7-hexahydro-3H-indazol-3-one

HRID 1762988
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HRID 1762988 반응식
[F:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([OH:9])=[CH:4][C:3]=1[NH:10][NH2:11].C([O:14][C:15]([CH:17]1[CH2:22][CH2:21][CH2:20][CH2:19][C:18]1=O)=O)C>C(O)(=O)C>[Cl:8][C:6]1[C:5]([OH:9])=[CH:4][C:3]([N:10]2[C:15](=[O:14])[CH:17]3[C:18]([CH2:19][CH2:20][CH2:21][CH2:22]3)=[N:11]2)=[C:2]([F:1])[CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 95543Ethyl 2-oxocyclohexanecarboxylateHCID 1850812-Chloro-4-fluoro-5-hydrazinylphenol

생성물 1

HCID 137530592-(4-Chloro-2-fluoro-5-hydroxyphenyl)-2,3a,4,5,6,7-hexahydro-3H-indazol-3-one수율 85.9%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A solution of 2-fluoro-4-chloro-5-hydroxyphenylhydrazine (8 g) and 2-ethoxycarbonylcyclohexanone (8 g) in acetic acid (30 ml) was heated under reflux for 4 hours. After cooling, the precipitated crystals were collected by filtration and washed with ether to give 11 g of 2-(4-chloro-2-fluoro-5-hydroxyphenyl)-2,3a,4,5,6,7-hexahydroindazol-3-one. m.p., 273°-275° C. (decomp.).

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후처리

  1. temperatureunder reflux for 4 hours
  2. temperatureAfter cooling
  3. filtrationthe precipitated crystals were collected by filtration
  4. washwashed with ether

출처 및 근거

ORD 기록
ord-177b15d30f9d4fd3b40c76c3dfc2de4b
출처 데이터셋
uspto-grants-1989_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04835286

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