Sodium Azide → HCID 86691397, Verbindung

HRID 540167Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 540167
Br[C:2]([CH3:31])([CH3:30])[C:3]([NH:5][C:6]1[C:15]2[C:10](=[CH:11][CH:12]=[C:13]([CH3:16])[CH:14]=2)[N:9]=[C:8]([N:17]2[CH2:23][C:22]3[CH:24]=[CH:25][CH:26]=[CH:27][C:21]=3[S:20](=[O:29])(=[O:28])[CH2:19][CH2:18]2)[CH:7]=1)=[O:4].[N-:32]=[N+:33]=[N-:34].[Na+]>C(#N)C>[N:32]([C:2]([CH3:31])([CH3:30])[C:3]([NH:5][C:6]1[C:15]2[C:10](=[CH:11][CH:12]=[C:13]([CH3:16])[CH:14]=2)[N:9]=[C:8]([N:17]2[CH2:23][C:22]3[CH:24]=[CH:25][CH:26]=[CH:27][C:21]=3[S:20](=[O:29])(=[O:28])[CH2:19][CH2:18]2)[CH:7]=1)=[O:4])=[N+:33]=[N-:34]

Komponenten

4

Edukt 2

HCID 33557Sodium AzideHCID 71255527HCID 71255527, Verbindung

Produkt 1

HCID 86691397HCID 86691397, VerbindungAusbeute 108 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

To a solution of 2-bromo-N-[2-(1,1-dioxido-2,3-dihydro-1,4-benzothiazepin-4(5H)-yl)-6-methylquinolin-4-yl]-2-methylpropanamide (160 mg, 0.319 mmol) in actonitrile (15 mL) was added sodium azide (62 mg, 0.958 mmol). After being refluxed overnight, the resulting mixture was concentrated in vacuo. The residue was diluted with ethyl acetate (40 mL), washed with brine, dried over sodium sulfate, and concentrated in vacuo to afford 160 mg of the crude product.

Aufarbeitung

  1. temperatureAfter being refluxed overnight
  2. concentrationthe resulting mixture was concentrated in vacuo
  3. additionThe residue was diluted with ethyl acetate (40 mL)
  4. washwashed with brine
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-2fc755a394b649ddaa64a7a89aede010
Quelldatensatz
uspto-grants-2014_10
Patentnummer
US08871756B2

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