Acetic Acid → HCID 2775935, Verbindung

HRID 635801Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 635801
[S:1]=[C:2]1[CH:7]=[N:6][NH:5][C:4](=[O:8])[NH:3]1.CI.[OH-].[Na+].[C:13](O)(=O)C>O>[CH3:13][S:1][C:2]1[CH:7]=[N:6][NH:5][C:4](=[O:8])[N:3]=1

Komponenten

6

Edukt 4

HCID 176Acetic AcidHCID 6328Methyl iodideHCID 14798Sodium HydroxideHCID 14162865-Thioxo-4,5-dihydro-1,2,4-triazin-3(2H)-one

Produkt 1

HCID 2775935HCID 2775935, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

The compound 9a (30 g, 232 mmol) and CH3I (15.9 ml, 255 mmol) are placed in 300 ml of water. 18.6 g of NaOH (465 mmol) are added and the mixture is stirred for 1 h at room temperature. The reaction mixture, cooled on a bed of ice, is neutralized using 27 ml of acetic acid and then extracted with dichloromethane. The organic phases are dried (MgSO4) and then concentrated to dryness. After recrystallizing from ether, 29.9 g of compound 9b are isolated.

Aufarbeitung

  1. temperatureThe reaction mixture, cooled on a bed of ice
  2. extractionextracted with dichloromethane
  3. dry with materialThe organic phases are dried (MgSO4)
  4. concentrationconcentrated to dryness
  5. customAfter recrystallizing from ether, 29.9 g of compound 9b
  6. customare isolated

Quellen und Nachweise

ORD-Eintrag
ord-727fbd0710e5469f87d70ea172070feb
Quelldatensatz
uspto-grants-2001_02
Patentnummer
US06191130B1

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