Hydrochloric Acid → Piperidine-4-carboxylic acid [6-(2-methoxy-phenyl)-pyrimidin-4-yl]-amide hydrochloride

HRID 1020050Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1020050
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9]1[N:14]=[CH:13][N:12]=[C:11]([NH:15][C:16]([CH:18]2[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]2)=[O:17])[CH:10]=1.[ClH:24]>O1CCOCC1>[ClH:24].[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9]1[N:14]=[CH:13][N:12]=[C:11]([NH:15][C:16]([CH:18]2[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]2)=[O:17])[CH:10]=1

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 59508946Piperidine-4-carboxylic acid [6-(2-methoxy-phenyl)-pyrimidin-4-yl]amide

Produkt 1

HCID 67184524Piperidine-4-carboxylic acid [6-(2-methoxy-phenyl)-pyrimidin-4-yl]-amide hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

Piperidine-4-carboxylic acid [6-(2-methoxy-phenyl)-pyrimidin-4-yl]amide (compound #6A) (2.0 g, 6.4 mmol) was dissolved in a saturated solution of HCl in 1,4-dioxane (50 ml) and the clear solution was stirred at room temperature for half an hour. A pale yellow solid precipitated out. Diethyl ether (50 ml) was added to precipitate more of the solid. After filtration, the solid was washed with diethyl ether (50 ml) and dried under high vacuum to obtain piperidine-4-carboxylic acid [6-(2-methoxy-phenyl)-pyrimidin-4-yl]-amide hydrochloride (compound #14A, HCl salt of compound #6A), 2.2 g, 98%) as a white solid.

Aufarbeitung

  1. customA pale yellow solid precipitated out
  2. additionDiethyl ether (50 ml) was added
  3. customto precipitate more of the solid
  4. filtrationAfter filtration
  5. washthe solid was washed with diethyl ether (50 ml)
  6. customdried under high vacuum

Quellen und Nachweise

ORD-Eintrag
ord-456c0ffd3ce74494b385458eda4ab5fc
Quelldatensatz
uspto-grants-2014_05
Patentnummer
US08716296B2

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