Dimethylformamide → HCID 74397972, Verbindung

HRID 1526289

Reaktionsgleichung

Reaktionsgleichung von HRID 1526289
[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[NH:8][C:9](=[O:14])[CH2:10][C:11](=[O:13])[CH3:12].C(=O)([O-])[O-].[K+].[K+].[CH3:21][N:22]([CH3:25])[CH:23]=O.COC(OC)N(C)C>O>[CH3:21][N:22]([CH:25]=[C:10]([C:11](=[O:13])[CH3:12])[C:9]([NH:8][C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=1[CH3:1])=[O:14])[CH3:23]

Komponenten

6

Edukt 4

HCID 6228DimethylformamideHCID 71542'-MethylacetoacetanilideHCID 11430Potassium CarbonateHCID 78373Dimethylformamide dimethyl acetal

Produkt 1

HCID 74397972HCID 74397972, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

To a mixture of N-(2-methylphenyl)-3-oxobutanamide (10.0 g), potassium carbonate (7.23 g) and N,N-dimethylformamide (130 mL) was added dropwise 1,1-dimethoxy-N,N-dimethylmethanamine (12.5 g) over 30 min at room temperature, and the reaction mixture was stirred at room temperature for 2 hr. The reaction mixture was slowly poured into water, and the mixture was extracted with dichloromethane. The extract was washed with water, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (10.2 g).

Aufarbeitung

  1. extractionthe mixture was extracted with dichloromethane
  2. washThe extract was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customthe solvent was evaporated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane)

Quellen und Nachweise

ORD-Eintrag
ord-423b8b9b926a4ed7bcfb3e0a69db0862
Quelldatensatz
uspto-grants-2015_07
Patentnummer
US09085578B2

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