Hydrazinecarbothioamide, N-phenyl- → 3-Anilino-4-acetyl-5-methylpyrazole

HRID 223416

Reaktionsgleichung

Reaktionsgleichung von HRID 223416
[C:1]1([NH:7][C:8](=S)[NH:9][NH2:10])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl[CH2:13][C:14]([CH2:16][C:17](=O)[CH3:18])=[O:15]>O1CCCC1>[NH:7]([C:8]1[C:16]([C:14](=[O:15])[CH3:13])=[C:17]([CH3:18])[NH:10][N:9]=1)[C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

Komponenten

4

Edukt 2

HCID 730679Hydrazinecarbothioamide, N-phenyl-HCID 144968561-Chloro-2,4-pentanedione

Produkt 1

HCID 204753773-Anilino-4-acetyl-5-methylpyrazole

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

50 g of 4-phenylthiosemicarbazide is suspended in 300 ml of tetrahydrofuran and 0.5 ml of concentrated HCL is added. Then 40.4 g of 3-chloroacetyl acetone is allowed to run in all at once and the whole is cooled with an ice-bath. After 12 hours' stirring, the precipitate formed is suction filtered, washed with acetone and then boiled in a water/acetone mixture (1:1). This hot solution is filtered off from the sulfur and neutralized with aqueous ammonia solution. The product is then suction filtered and recrystallized from acetone; m.p. 246°-247° C.

Aufarbeitung

  1. addition0.5 ml of concentrated HCL is added
  2. temperatureis cooled with an ice-bath
  3. customthe precipitate formed
  4. filtrationfiltered
  5. washwashed with acetone
  6. filtrationThis hot solution is filtered off from the sulfur and neutralized with aqueous ammonia solution
  7. filtrationsuction filtered
  8. customrecrystallized from acetone

Quellen und Nachweise

ORD-Eintrag
ord-571d4729c84c4820b9fa50bf881db780
Quelldatensatz
uspto-grants-1982_10
Patentnummer
US04354031

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