Ammonia → 4-Isopropoxy-3-thioureidobenzenesulfonamide

HRID 405674Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 405674
[CH:1]([O:4][C:5]1[CH:10]=[CH:9][C:8]([S:11]([NH2:14])(=[O:13])=[O:12])=[CH:7][C:6]=1[N:15]=[C:16]=[S:17])([CH3:3])[CH3:2].[NH3:18]>CO>[CH:1]([O:4][C:5]1[CH:10]=[CH:9][C:8]([S:11]([NH2:14])(=[O:13])=[O:12])=[CH:7][C:6]=1[NH:15][C:16]([NH2:18])=[S:17])([CH3:3])[CH3:2]

Komponenten

4

Edukt 2

HCID 222AmmoniaHCID 866653704-Isopropoxy-3-isothiocyanato-benzenesulfonamide

Produkt 1

HCID 866655834-Isopropoxy-3-thioureidobenzenesulfonamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

Crude 4-isopropoxy-3-isothiocyanato-benzenesulfonamide (17.8 g, 65.2 mmol, example 2, step e) was treated with a 2 M solution of ammonia in MeOH (250 mL) and the resulting solution was stirred at room temperature for 18 h. The reaction mixture was then concentrated to about half the volume until a large amount of tan solid precipitated. The suspension was cooled to 0° C. for 30 minutes and was filtered. The solid was washed with methanol and ether to give the title compound as a cream colored solid.

Aufarbeitung

  1. concentrationThe reaction mixture was then concentrated to about half the volume until a large amount of tan solid
  2. customprecipitated
  3. temperatureThe suspension was cooled to 0° C. for 30 minutes
  4. filtrationwas filtered
  5. washThe solid was washed with methanol and ether

Quellen und Nachweise

ORD-Eintrag
ord-0f5602def9e44f86b5b52862fec149a9
Quelldatensatz
uspto-grants-2014_06
Patentnummer
US08753857B2

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