Iodine → HCID 178471365, Verbindung

HRID 1055182

Reaktionsgleichung

Reaktionsgleichung von HRID 1055182
[Zn:1].II.[Br:4]CCCCCCCCC(OCC)=O.[C:18]([O:28][CH2:29][CH3:30])(=[O:27])[CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26]>CC(N(C)C)=O>[Br:4][Zn:1][CH2:26][CH2:25][CH2:24][CH2:23][CH2:22][CH2:21][CH2:20][CH2:19][C:18]([O:28][CH2:29][CH3:30])=[O:27]

Komponenten

6

Edukt 4

HCID 807Iodine2×HCID 23994Zinc2×HCID 31251Ethyl NonanoateHCID 560317Disodium acetylide

Produkt 1

HCID 178471365HCID 178471365, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 31374DimethylacetamideLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

In a dry reaction tube under nitrogen were charged zinc dust (3.70 g, 56.6 mmol), iodine (479 mg, 1.89 mmol) and dry DMA (20 mL). The mixture was stirred at room temperature until the color of iodine disappeared. Ethyl 9-bromononanoate was added, and the mixture was stirred at 80° C. for 4 hours and then at room temperature overnight. (Completion of the zinc insertion reaction was checked by GCMS analysis of the hydrolyzed reaction mixture.) The reaction mixture was used without further treatment in the subsequent step. GCMS m/z 186 [M]+ (ethyl nonanoate).

Aufarbeitung

  1. customIn a dry reaction tube under nitrogen
  2. customat room temperature
  3. customovernight

Quellen und Nachweise

ORD-Eintrag
ord-0ef785149a124889a3ddb5d4f53c3659
Quelldatensatz
uspto-grants-2016_07
Patentnummer
US09393315B2

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