Methylhydrazine → N-(2-benzoyl-4-chlorophenyl)-methyl-hydrazinecarbothioamide

HRID 26641

Reaktionsgleichung

Reaktionsgleichung von HRID 26641
[C:1]([C:9]1[CH:14]=[C:13]([Cl:15])[CH:12]=[CH:11][C:10]=1[N:16]=[C:17]=[S:18])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:19][NH:20][NH2:21].[N-]=C=S>C(OCC)C>[C:1]([C:9]1[CH:14]=[C:13]([Cl:15])[CH:12]=[CH:11][C:10]=1[NH:16][C:17]([N:20]([CH3:19])[NH2:21])=[S:18])(=[O:8])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

Komponenten

5

Edukt 3

HCID 6061MethylhydrazineHCID 5200219Sbb012730HCID 178418790HCID 178418790, Verbindung

Produkt 1

HCID 13972523N-(2-benzoyl-4-chlorophenyl)-methyl-hydrazinecarbothioamideAusbeute 91 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel3×

Versuchsvorschrift

A solution of 5.48 grams (0.02 mole) of 2-benzoyl-4-chlorophenylisothiocyanate in about 50 ml of ethyl ether was added dropwise to a solution containing 1.5 ml (0.028 mole) of methyl hydrazine (98%) in about 50 ml of ethyl ether cooled in an ice bath. Additional ethyl ether was added to facilitate stirring. Following addition of the isothiocyanate, the reaction mixture was stirred at room temperature for about 30 minutes. The solid was collected and washed with additional ethyl ether to yield 5.82 grams (91% yield) of N-(2-benzoyl-4-chlorophenyl)-methyl-hydrazinecarbothioamide as a white solid. The melting point was found to be 168.5°-170° C.

Aufarbeitung

  1. temperaturecooled in an ice bath
  2. stirringthe reaction mixture was stirred at room temperature for about 30 minutes
  3. customThe solid was collected
  4. washwashed with additional ethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-e790afca29034886892401cfb6b13f60
Quelldatensatz
uspto-grants-1979_04
Patentnummer
US04151166

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