Acetic Acid → HCID 13687198, Verbindung

HRID 651899

Reaktionsgleichung

Reaktionsgleichung von HRID 651899
[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

Komponenten

5

Edukt 3

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

Produkt 1

HCID 13687198HCID 13687198, VerbindungAusbeute 39,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 7237O-XyleneLösungsmittel

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-106cbea6a88b4b63a8367ed8573521be
Quelldatensatz
uspto-grants-1987_06
Patentnummer
US04670043

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