Acetic Acid → HCID 13687198、化合物

HRID 651899

反応式

HRID 651899 の反応式
[Cl:1][C:2]1[C:7]([O:8][CH:9]([CH3:11])[CH3:10])=[CH:6][C:5]([NH:12][NH2:13])=[C:4]([F:14])[CH:3]=1.[C:15]([CH:18]1[CH2:23][CH2:22][CH2:21][CH2:20][C:19]1=O)(=O)[CH3:16].C(O)(=O)C>C1(C)C(C)=CC=CC=1>[CH3:16][C:15]1[N:12]([C:5]2[CH:6]=[C:7]([O:8][CH:9]([CH3:10])[CH3:11])[C:2]([Cl:1])=[CH:3][C:4]=2[F:14])[N:13]=[C:19]2[C:18]=1[CH2:23][CH2:22][CH2:21][CH2:20]2

参加物

5

反応物 3

HCID 176Acetic AcidHCID 134002-AcetylcyclohexanoneHCID 185080(4-Chloro-2-fluoro-5-propan-2-yloxyphenyl)hydrazine

生成物 1

HCID 13687198HCID 13687198、化合物収率 39.1%

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

実験手順

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.

後処理

  1. temperatureunder reflux for 8 hours
  2. customwhile removing water
  3. temperatureAfter cooling
  4. concentrationthe reaction mixture was concentrated under reduced pressure
  5. customthe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-106cbea6a88b4b63a8367ed8573521be
出典データセット
uspto-grants-1987_06
特許番号
US04670043

関連ノート

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