Reaktion #65409

Reaktionsgleichung

α-acetyl-4-phenylthiophenylacetonitrile

semicarbazide hydrochloride

methanol

→

title compound

Ausbeute 91.4%

3-Amino-5-methyl-4-(4-phenylthiophenyl)pyrazole

Ausbeute 91.4%

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeRemoving the ice bath, 40 hours later
2. 2
   workup.STIRRINGthe mixture was stirred at room temperature for 1 hour
3. 3
   workup.ADDITIONAdding 50 ml of water
4. 4
   workup.STIRRINGthe mixture was stirred for 30 minutes in ice-
5. 5
   Temperaturcooling
6. 6
   Filtrationthe precipitate was filtered
7. 7
   workup.ADDITIONIt was directly added to the mixed solution of 5 ml of aqueous solution of 2N sodium hydroxide and 50 ml of methanol
8. 8
   workup.STIRRINGthe mixture was stirred for 4 hours at room temperature
9. 9
   workup.ADDITION80 ml of water was added
10. 10
    workup.STIRRINGthe mixture was stirred for 30 minutes in ice-
11. 11
    Temperaturcooling
12. 12
    Filtrationthe precipitate was filtered
13. 13
    WaschenWashed in water
14. 14
    Sonstigedried

Vorschrift

A mixture of 520 mg of α-acetyl-4-phenylthiophenylacetonitrile, 217 mg of semicarbazide hydrochloride, 15 ml of methanol and 3 ml of water was stirred at 0° C. for 10 minutes. Removing the ice bath, 40 hours later, the mixture was stirred at room temperature for 1 hour while keeping the pH at 9 to 10 by using aqueous solution of 2N sodium hydroxide. Adding 50 ml of water, the mixture was stirred for 30 minutes in ice-cooling, and the precipitate was filtered. It was directly added to the mixed solution of 5 ml of aqueous solution of 2N sodium hydroxide and 50 ml of methanol, and the mixture was stirred for 4 hours at room temperature, and then 80 ml of water was added, and the mixture was stirred for 30 minutes in ice-cooling, then the precipitate was filtered, Washed in water and dried, thereby obtaining 500 mg of the title compound.

Quelle