Hydrochloric Acid → Picolinimidamide

HRID 1484869

Reaktionsgleichung

Reaktionsgleichung von HRID 1484869
[Li+].C[Si]([N-:6][Si](C)(C)C)(C)C.[N:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[C:17]#[N:18].Cl>>[N:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[C:17](=[NH:6])[NH2:18]

Komponenten

4

Edukt 3

HCID 313Hydrochloric AcidHCID 7522Pyridine-2-carbonitrileHCID 2733832Lithium Hexamethyldisilazide

Produkt 1

HCID 556504PicolinimidamideAusbeute 82.549,203 %

Versuchsvorschrift

To the solution of LiHMDS (5.18 g, 0.026 mmol, 1.3 equiv.) was added picolinonitrile (2.08 g, 0.02 mmol, 1 equiv.) at ice-bath and kept stirred for 2 h. Then, the reaction mixture was acidified with aqueous HCl (4N) to pH2, cooled at ice-bath and kept stirred. Then, the mixture was extracted with EA (200 mL×5). The combined organic phase was washed with brine, dried (Na2SO4), and evaporated to get picolinimidamide (2.0 g, 83%). LC-MS (m/z)=122 [M+H]+.

Aufarbeitung

  1. temperaturecooled at ice-bath
  2. stirringkept stirred
  3. extractionThen, the mixture was extracted with EA (200 mL×5)
  4. washThe combined organic phase was washed with brine
  5. dry with materialdried (Na2SO4)
  6. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-173bb4f0572f44d6a2f2284180ab7a71
Quelldatensatz
uspto-grants-2016_08
Patentnummer
US09422271B2

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