Hydrochloric Acid → 6-[(2-Aminoethyl)amino]nicotinonitrile dihydrochloride

HRID 444810

Reaktionsgleichung

Reaktionsgleichung von HRID 444810
[C:1]([C:3]1[CH:4]=[CH:5][C:6]([NH:9][CH2:10][CH2:11][NH:12]C(=O)OC(C)(C)C)=[N:7][CH:8]=1)#[N:2].[ClH:20]>O1CCOCC1>[ClH:20].[ClH:20].[NH2:12][CH2:11][CH2:10][NH:9][C:6]1[CH:5]=[CH:4][C:3]([C:1]#[N:2])=[CH:8][N:7]=1

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 47453716tert-Butyl (2-((5-cyanopyridin-2-yl)amino)ethyl)carbamate

Produkt 1

HCID 669113296-[(2-Aminoethyl)amino]nicotinonitrile dihydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

7.9 g (30 mmol) of tert-butyl {2-[(5-cyanopyridin-2-yl)amino]ethyl}carbamate (Example 1A) were dissolved in 100 ml of 4N hydrogen chloride in dioxane and the mixture was stirred for 30 min. The reaction mixture was concentrated to half of its original volume and the same amount of diethyl ether was added. The reaction mixture was stirred for 20 min and the product was filtered off and washed with diethyl ether. This gave 7 g (94% of theory) of the product as a solid.

Aufarbeitung

  1. concentrationThe reaction mixture was concentrated to half of its original volume
  2. additionthe same amount of diethyl ether was added
  3. stirringThe reaction mixture was stirred for 20 min
  4. filtrationthe product was filtered off
  5. washwashed with diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-43f92318cda642ed868838c8d8031caf
Quelldatensatz
uspto-grants-2013_07
Patentnummer
US08476267B2

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