O-Xylene → 2-(4-chloro-2-fluorophenyl)-3-methyl-4,5,6,7-tetrahydro-2H-indazole

HRID 1703444ノート

反応式

HRID 1703444 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][NH2:9])=[C:4]([F:10])[CH:3]=1.[C:11]([CH:14]1[CH2:19][CH2:18][CH2:17][CH2:16][C:15]1=O)(=O)[CH3:12].C1(C)C(C)=CC=CC=1>C(O)(=O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:11]([CH3:12])=[C:14]3[C:15]([CH2:16][CH2:17][CH2:18][CH2:19]3)=[N:9]2)=[C:4]([F:10])[CH:3]=1

参加物

5

反応物 3

HCID 7237O-XyleneHCID 134002-AcetylcyclohexanoneHCID 2782934(4-Chloro-2-fluorophenyl)hydrazine

生成物 1

HCID 212012922-(4-chloro-2-fluorophenyl)-3-methyl-4,5,6,7-tetrahydro-2H-indazole

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A solution of 19.7 parts of 4-chloro-2-fluorophenylhydrazine and 14.0 parts of 2-acetylcyclohexanone in 50 parts of xylene and 1 part of glacial acetic acid were refluxed for 24 hours with a Dean Stark trap to collect the water formed. The xylene was distilled from the mixture. The residual oil was dissolved in arm hexane solution. On cooling, 6.2 parts of crude product was obtained. Recrystallization of this product yielded white crystals of 2-(4-chloro-2-fluorophenyl)-3-methyl-4,5,6,7-tetrahydro-2H-indazole, melting point 84.5°-87.5° C; ir bands (1570 cm-1, 905 cm-1, 822 cm-1).

後処理

  1. customto collect the water
  2. customformed
  3. distillationThe xylene was distilled from the mixture
  4. dissolutionThe residual oil was dissolved in arm hexane solution
  5. temperatureOn cooling
  6. custom6.2 parts of crude product was obtained
  7. customRecrystallization of this product

出典と根拠

ORDレコード
ord-e1c1d5515edd487ab21f4946fcf04def
出典データセット
uspto-grants-1978_11
特許番号
US04124374

反応ノート

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