Acetone → HCID 178482503, Verbindung

HRID 67726

Reaktionsgleichung

Reaktionsgleichung von HRID 67726
[CH3:1][NH:2][C:3](=[S:6])[NH:4][NH2:5].CC(C)=O.N1[CH:16]=[CH:15][CH:14]=CC=1.[C:17](Cl)(=[O:22])[C:18]([CH3:21])([CH3:20])[CH3:19]>O>[CH3:1][NH:2][C:3]1[S:6][C:15]([CH3:14])([CH3:16])[N:5]([C:17](=[O:22])[C:18]([CH3:21])([CH3:20])[CH3:19])[N:4]=1

Komponenten

6

Edukt 4

HCID 180AcetoneHCID 1049PyridineHCID 62493Pivaloyl chlorideHCID 2723853N-Methylhydrazinecarbothioamide

Produkt 1

HCID 178482503HCID 178482503, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A 52.5 g. portion of 4-methylthiosemicarbazide was suspended and partially dissolved in 250 ml. of acetone, and 39.5 g. of pyridine was added. The mixture was stirred for 15 minutes at ambient temperature, and then 60.5 g. of pivaloyl chloride was added slowly while the temperature of the reaction mixture was held at 20°-25°. The mixture was stirred at ambient temperature for 3 hours after the addition, and then 200 ml. of water was added. The reaction mixture was filtered, and the filter cake was washed with 100 ml. of nitromethane and vacuum dried at 50° to obtain 91.4 g. of the desired intermediate product, m.p. 162°-164°.

Aufarbeitung

  1. dissolutionpartially dissolved in 250 ml
  2. customwas held at 20°-25°
  3. stirringThe mixture was stirred at ambient temperature for 3 hours
  4. additionafter the addition
  5. filtrationThe reaction mixture was filtered
  6. washthe filter cake was washed with 100 ml
  7. dry with materialof nitromethane and vacuum dried at 50°
  8. customto obtain 91.4 g

Quellen und Nachweise

ORD-Eintrag
ord-4b7df4c1a3284005a4e7170acdd589a1
Quelldatensatz
uspto-grants-1982_08
Patentnummer
US04346225

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