Hydrochloric Acid → HCID 178491370, Verbindung

HRID 447941

Reaktionsgleichung

Reaktionsgleichung von HRID 447941
Cl.[CH3:2][O:3][C:4]1[CH:11]=[CH:10][CH:9]=[C:8]([O:12][CH3:13])[C:5]=1[CH2:6][NH2:7].[N-:14]([C:17]#[N:18])[C:15]#[N:16].[Na+]>>[C:15]([NH:14][C:17]([NH:7][CH2:6][C:5]1[C:8]([O:12][CH3:13])=[CH:9][CH:10]=[CH:11][C:4]=1[O:3][CH3:2])=[NH:18])#[N:16]

Komponenten

4

Versuchsvorschrift

15 ml 2N hydrochloric acid were added to 5.0 g (29.9 mmol) 2,6-dimethoxybenzylamine and the aqueous phase was subsequently removed under vacuum. The residue was then dissolved in 50 ml 1-butanol and 2.66 g (29.9 mmol) of sodium dicyanamide were added. The reaction mixture was heated for 5.5 hours at reflux and stirred for 12 hours at room temperature. The precipitate formed was filtered off, was washed with diethylether; 6.81 g.

Aufarbeitung

  1. customthe aqueous phase was subsequently removed under vacuum
  2. dissolutionThe residue was then dissolved in 50 ml 1-butanol
  3. temperatureThe reaction mixture was heated for 5.5 hours
  4. temperatureat reflux
  5. customThe precipitate formed
  6. filtrationwas filtered off
  7. washwas washed with diethylether

Quellen und Nachweise

ORD-Eintrag
ord-0740ffcdbd084f38a1576fed031345a4
Quelldatensatz
uspto-grants-2013_07
Patentnummer
US08481576B2

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