Ammonium Chloride → HCID 22678484, Verbindung

HRID 1837690Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1837690
[CH3:1][O:2][C:3]1[C:8]([CH2:9][N:10]2[CH2:15][CH2:14][CH:13]([CH:16]=[C:17](Br)Br)[CH2:12][CH2:11]2)=[CH:7][CH:6]=[CH:5][N:4]=1.CCCCCC.C([Li])CCC.[Cl-].[NH4+]>O1CCCC1>[CH3:1][O:2][C:3]1[C:8]([CH2:9][N:10]2[CH2:15][CH2:14][CH:13]([C:16]#[CH:17])[CH2:12][CH2:11]2)=[CH:7][CH:6]=[CH:5][N:4]=1

Komponenten

5

Edukt 3

HCID 25517Ammonium ChlorideHCID 226784931-[(2-Methoxy-3-piridyl)methyl]-4-(2,2-dibromovinyl)piperidineHCID 178418244HCID 178418244, Verbindung

Produkt 1

HCID 22678484HCID 22678484, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Reaktionsbedingungen

Temperatur
-78 °C

Versuchsvorschrift

2.9 g of 1-[(2-methoxy-3-piridyl)methyl]-4-(2,2-dibromovinyl)piperidine was dissolved in 25 ml of tetrahydrofuran, and 12.3 ml of a 1.50 M n-butyllithium hexane solution was added dropwise at −78° C. After completing the dropwise addition, the mixture was further stirred at −78° C. for one hour. An aqueous saturated ammonium chloride was added to the reaction solution, and the mixture was extracted with ethyl acetate. The organic layer was washed with brine, and then the dried over anhydrous magnesium sulfate. The solvent was evaporated, to give the title compound as a yellow oil (quantitatively).

Aufarbeitung

  1. additionthe dropwise addition
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe organic layer was washed with brine
  4. dry with materialthe dried over anhydrous magnesium sulfate
  5. customThe solvent was evaporated

Quellen und Nachweise

ORD-Eintrag
ord-7870dfc4cc154e88ba2ddb0bdef3fb80
Quelldatensatz
uspto-grants-2004_08
Patentnummer
US06784192B2

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