Triethylamine → HCID 131737089, Verbindung

HRID 60383Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 60383
[Br:1][C:2]1[O:6][C:5]([CH:7]=[CH:8][C:9]([OH:11])=O)=[CH:4][CH:3]=1.C(N(CC)CC)C.ClC(OCC)=O.[N-:25]=[N+:26]=[N-:27].[Na+]>C(#N)C>[Br:1][C:2]1[O:6][C:5]([CH:7]=[CH:8][C:9]([N:25]=[N+:26]=[N-:27])=[O:11])=[CH:4][CH:3]=1

Komponenten

6

Edukt 4

HCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 33557Sodium AzideHCID 9460883-(5-Bromofuran-2-yl)prop-2-enoic acid

Produkt 1

HCID 131737089HCID 131737089, VerbindungAusbeute 44,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

To a solution of 3-(5-bromo-2-furyl)acrylic acid (41.5 g) in acetonitrile (200 mL) were added triethylamine (23.0 g) and ethyl chloroformate (26.1 g). The mixture was stirred at room temperature for 30 min. To the obtained mixture was added a saturated aqueous solution of sodium azide (18.7 g) at 0° C. and the mixture was stirred at room temperature for 5 hr. The reaction mixture was filtered, and the obtained solid was washed with water. The solid was recrystallized from dichloromethane to give the title compound (20.7 g) as white solid.

Aufarbeitung

  1. stirringthe mixture was stirred at room temperature for 5 hr
  2. filtrationThe reaction mixture was filtered
  3. washthe obtained solid was washed with water
  4. customThe solid was recrystallized from dichloromethane

Quellen und Nachweise

ORD-Eintrag
ord-f311bd1396044febb1d35e93ccc5e430
Quelldatensatz
uspto-grants-2016_09
Patentnummer
US09440987B2

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