Sodium Azide → HCID 16748734, Verbindung

HRID 457574

Reaktionsgleichung

Reaktionsgleichung von HRID 457574
[Br:1][C:2]1[CH:3]=[C:4]([CH:9]=[CH:10][CH:11]=1)[C:5](=[O:8])[CH2:6]Br.[N-:12]=[N+:13]=[N-:14].[Na+]>CO>[Br:1][C:2]1[CH:3]=[C:4]([CH:9]=[CH:10][CH:11]=1)[C:5](=[O:8])[CH2:6][N:12]=[N+:13]=[N-:14]

Komponenten

4

Edukt 2

HCID 33557Sodium AzideHCID 5195852-Bromo-1-(3-bromophenyl)ethan-1-one

Produkt 1

HCID 16748734HCID 16748734, VerbindungAusbeute 99,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

A solution of 20.2 g (73 mmol) of 3-bromophenacyl bromide and 5.42 g (83 mmol) of sodium azide was stirred at RT for 90 min in methanol. The solvent was removed under reduced pressure and the crude product was partitioned between ethyl acetate (200 ml) and water (100 mL). The organic layer was separated, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to afford the title compound (17.4 g, 99%) as a light yellow solid. 1H NMR (400 MHz, d6-DMSO): δ 8.10 (d, J=1.0, 1H), 7.90–7.97 (m, 2H), 7.22 (t, J=7.9, 1H), 4.93 (s, 2H).

Aufarbeitung

  1. customThe solvent was removed under reduced pressure
  2. customthe crude product was partitioned between ethyl acetate (200 ml) and water (100 mL)
  3. customThe organic layer was separated
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-04496d367c7b4f678864836d4b3ee3b1
Quelldatensatz
uspto-grants-2007_03
Patentnummer
US07189712B2

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