Methyl isothiocyanate → HCID 178488243, Verbindung

HRID 500544Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 500544
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:10]=[CH:11][N:12]=1)[C:6]([NH:8][NH2:9])=O.[CH3:13][N:14]=[C:15]=[S:16].[OH-].[Na+]>O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:6]2[N:14]([CH3:13])[C:15]([SH:16])=[N:9][N:8]=2)[CH:10]=[CH:11][N:12]=1

Komponenten

5

Edukt 3

HCID 11167Methyl isothiocyanateHCID 14798Sodium HydroxideHCID 3225512-Methoxyisonicotinohydrazide

Produkt 1

HCID 178488243HCID 178488243, VerbindungAusbeute 87 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

The title compound of example 23.1 (18.35 g, 109.8 mmol) and methyl isothiocyanate (8.83 g, 120 mmol) were stirred together at 60° C. for 30 minutes. Sodium hydroxide (4.83 g, 120 mmol) in water (32 mL) was added to the reaction mixture it was allowed to continue to stir at 60° C. for 12 hours. The reaction mixture was concentrated and diluted with water. It was acidified to pH 4-5 with 3 M HCl. A solid precipitated out which was filtered, washing with portions of water, then dried to afford the product as a beige solid (21.2 g, 87%).

Aufarbeitung

  1. concentrationThe reaction mixture was concentrated
  2. additiondiluted with water
  3. customA solid precipitated out which
  4. filtrationwas filtered
  5. washwashing with portions of water
  6. customdried

Quellen und Nachweise

ORD-Eintrag
ord-c51b3d4008d2404abf5a551ade3cdcf0
Quelldatensatz
uspto-grants-2010_08
Patentnummer
US07772235B2

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