Dimethylformamide → HCID 178510459, Verbindung

HRID 1985663Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1985663
C(#N)C([CH2:4][C:5]#[N:6])O.[H-].[Na+].[N:10]1([C:16]2[CH:27]=[C:20]3[C:21]([O:23][C:24](=O)[NH:25][C:19]3=[CH:18][CH:17]=2)=O)[CH2:15][CH2:14][O:13][CH2:12][CH2:11]1.C[N:29](C)C=O>O>[NH2:29][C:24]1[C:4]([C:5]#[N:6])=[C:21]([OH:23])[C:20]2[C:19](=[CH:18][CH:17]=[C:16]([N:10]3[CH2:11][CH2:12][O:13][CH2:14][CH2:15]3)[CH:27]=2)[N:25]=1

Komponenten

6

Edukt 4

HCID 6228DimethylformamideHCID 24758Sodium hydrideHCID 212535622-HydroxybutanedinitrileHCID 866077765-(Morpholin-4-yl)isatoic anhydride

Produkt 1

HCID 178510459HCID 178510459, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

4 g of malonitrile is dissolved in 50 mL of dimethylformamide. To the solution, in several portions, 2.4 g of 60% oily dispersion of sodium hydride are added. To the clear solution 8 g of 5-(morpholin-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, the pH is adjusted to 6 with acetic acid. The precipitated material is filtered off, washed with water. After drying 6.5 g of the title compound is obtained, m.p.: 291° C.

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-bb3a9b1d90b641158c79b2500c34699c
Quelldatensatz
uspto-grants-2009_06
Patentnummer
US07547696B2

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