2-Chlorocyclohexanone → HCID 23312424, Verbindung

HRID 745756Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 745756
Cl.N[C:3]1CC[N:5]([C:8]2[S:9][C:10]3[CH2:16][CH2:15][CH2:14][CH2:13][C:11]=3[N:12]=2)[N:4]=1.C(NNC(N)=S)=[O:18].[Cl:24]C1CCCCC1=O>CN(C)C=O>[ClH:24].[CH:3]([NH:4][NH:5][C:8]1[S:9][C:10]2[CH2:16][CH2:15][CH2:14][CH2:13][C:11]=2[N:12]=1)=[O:18]

Komponenten

5

Edukt 3

HCID 132032-ChlorocyclohexanoneHCID 27754861-Formyl-3-thiosemicarbazideHCID 23312414HCID 23312414, Verbindung

Produkt 1

HCID 23312424HCID 23312424, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

The 2-hydrazino-4,5,6,7-tetrahydro-benzothiazole hydrochloride used above is prepared in accordance with the method of Y.Usui [CA 70,96685 (1969)] via Hantzsch synthesis, with better yields by modification of the conditions. A mixture of 20 g of formylthiosemicarbazide, 22.3 g of 2-chlorocyclohexanone and 150 ml of dimethylformamide is kept at 70°-80° C. for 3 hours. On cooling, some of the product crystallises out. The dimethylformamide is distilled off in vacuo and the residue is recrystallised from ethanol. 27.4 g of 1-formyl-2-(4,5,6,7-tetrahydro-benzothiazolyl)-hydrazine hydrochloride of melting point 171°-173° C. are obtained.

Aufarbeitung

  1. customabove is prepared in accordance with the method of Y.Usui [CA 70,96685 (1969)] via Hantzsch synthesis
  2. customwith better yields by modification of the conditions
  3. temperatureOn cooling
  4. customsome of the product crystallises out
  5. distillationThe dimethylformamide is distilled off in vacuo
  6. customthe residue is recrystallised from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-85e79c7c84a14e198a5d9b7ae9deefdc
Quelldatensatz
uspto-grants-1986_07
Patentnummer
US04600722

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