Lithium Hydroxide → N-(3,5-difluoro-benzyl)-2-methyl-malonamic acid

HRID 2223242Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2223242
C([O:3][C:4](=[O:19])[CH:5]([CH3:18])[C:6]([NH:8][CH2:9][C:10]1[CH:15]=[C:14]([F:16])[CH:13]=[C:12]([F:17])[CH:11]=1)=[O:7])C.[OH-].[Li+]>C(O)C.O>[F:16][C:14]1[CH:15]=[C:10]([CH:11]=[C:12]([F:17])[CH:13]=1)[CH2:9][NH:8][C:6](=[O:7])[CH:5]([CH3:18])[C:4]([OH:19])=[O:3]

Komponenten

5

Edukt 2

HCID 3939Lithium HydroxideHCID 69280082N-(3,5-Difluoro-benzyl)-2-methyl-malonamic acid ethyl ester

Produkt 1

HCID 21091473N-(3,5-difluoro-benzyl)-2-methyl-malonamic acid

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

To a solution of 4.0 g (14.75 mmol) N-(3,5-difluoro-benzyl)-2-methyl-malonamic acid ethyl ester in 300 ml of ethanol, 15 ml of water and 1.41 g (59 mmol) of lithium hydroxide were added and the mixture was refluxed for 5 hours. After concentration in vacuo water (50 ml) was added and the mixture was extracted with dichloromethane (three times 30 ml). The aqueous phase was acidified with 8 N hydrochloric acid and extracted with dichloromethane (four times 30 ml).

Aufarbeitung

  1. temperaturethe mixture was refluxed for 5 hours
  2. concentrationAfter concentration in vacuo water (50 ml)
  3. additionwas added
  4. extractionthe mixture was extracted with dichloromethane (three times 30 ml)
  5. extractionextracted with dichloromethane (four times 30 ml)

Quellen und Nachweise

ORD-Eintrag
ord-45e91b0a0d784d0c84933259972d1081
Quelldatensatz
uspto-grants-2008_05
Patentnummer
US07375099B2

Notizen zur Reaktion

Wird geladen…