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Dimethylformamide → HCID 178429869, Verbindung

HRID 2195688
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2195688
C(#N)C([CH2:4][C:5]#[N:6])O.[H-].[Na+].[CH3:10][CH:11]1[O:16][CH:15]([CH3:17])[CH2:14][N:13]([C:18]2[CH:29]=[C:22]3[C:23]([O:25][C:26](=O)[NH:27][C:21]3=[CH:20][CH:19]=2)=O)[CH2:12]1.C[N:31](C)C=O>O>[NH2:31][C:26]1[C:4]([C:5]#[N:6])=[C:23]([OH:25])[C:22]2[C:21](=[CH:20][CH:19]=[C:18]([N:13]3[CH2:14][CH:15]([CH3:17])[O:16][CH:11]([CH3:10])[CH2:12]3)[CH:29]=2)[N:27]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 6228DimethylformamideHCID 24758Sodium hydrideHCID 212535622-HydroxybutanedinitrileHCID 866445925-(2,6-Dimethylmorpholin-4-yl)isatoic anhydride

Produkt 1

HCID 178429869HCID 178429869, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962
Water
Lösungsmittel

Versuchsvorschrift

4 g of malonitrile is dissolved in 50 ml of dimethylformamide. To the solution, in several portions, 2.4 g of 60% sodium hydride in oily dispersion are added. To the clear solution 8 g of 5-(2,6-dimethylmorpholin-4-yl)isatoic anhydride is added and the mixture is stirred at room temperature for 10 hours. The reaction mixture is diluted with 70 ml of water and extracted with 2×30 ml of ethyl acetate. The aqueous phase is evaporated in vacuum, the solid residue is dissolved in 20 ml of water, and the pH is set to 6. The precipitated material is filtered off, washed with water. After drying 6.5 g of the title compound is obtained. (MH+: 299)

Aufarbeitung

  1. extractionextracted with 2×30 ml of ethyl acetate
  2. customThe aqueous phase is evaporated in vacuum
  3. dissolutionthe solid residue is dissolved in 20 ml of water
  4. filtrationThe precipitated material is filtered off
  5. washwashed with water
  6. dry with materialAfter drying 6.5 g of the title compound
  7. customis obtained

Quellen und Nachweise

ORD-Eintrag
ord-1406628a7fcb43afb1d23d682abba600
Quelldatensatz
uspto-grants-2012_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08338411B2

Notizen zur Reaktion

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