Ethanol → 3-Trifluoromethylbenzoic acid [1-(3-pyridinyl)propylidene]hydrazide

HRID 1085970Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1085970
[F:1][C:2]([F:14])([F:13])[C:3]1[CH:4]=[C:5]([CH:10]=[CH:11][CH:12]=1)[C:6]([NH:8][NH2:9])=[O:7].[CH2:15]([C:17]([C:19]1[CH:20]=[N:21][CH:22]=[CH:23][CH:24]=1)=O)[CH3:16].C(O)C>C(O)(=O)C.O>[N:21]1[CH:22]=[CH:23][CH:24]=[C:19]([C:17](=[N:9][NH:8][C:6](=[O:7])[C:5]2[CH:10]=[CH:11][CH:12]=[C:3]([C:2]([F:13])([F:14])[F:1])[CH:4]=2)[CH2:15][CH3:16])[CH:20]=1

Komponenten

6

Edukt 3

HCID 702EthanolHCID 740741-(3-Pyridyl)propan-1-oneHCID 27774173-(Trifluoromethyl)benzoic acid hydrazide

Produkt 1

HCID 540455043-Trifluoromethylbenzoic acid [1-(3-pyridinyl)propylidene]hydrazideAusbeute 74 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 176Acetic AcidKatalysatorHCID 962WaterLösungsmittel

Versuchsvorschrift

A mixture of 10.21 gm (0.05 mole) of 3-trifluoromethylbenzoic acid hydrazide, 6.76 gm (0.05 mole) of ethyl-3-pyridyl ketone, 10 drops of glacial acetic acid and 100 ml of absolute ethanol was refluxed 15 hr. The reaction mixture was diluted with water to the cloud point and cooled to room temperature then chilled in the refrigerator. The solids that separated were collected, washed with Skellysolve B and dried to give 11.88 gm (74%) of product having a melting point of 119.4° C.

Aufarbeitung

  1. temperaturewas refluxed 15 hr
  2. temperaturethen chilled in the refrigerator
  3. customThe solids that separated
  4. customwere collected
  5. washwashed with Skellysolve B
  6. customdried

Quellen und Nachweise

ORD-Eintrag
ord-2b4e538ebdce439b8fa05d5427632b7c
Quelldatensatz
uspto-grants-1991_04
Patentnummer
US05011932

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