Hydrochloric Acid → HCID 17976006, Verbindung

HRID 2264517Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2264517
N[C:2]1[C:7]([C:8]#[N:9])=[C:6]([C:10]2[CH:18]=[CH:17][C:13]3[O:14][CH2:15][O:16][C:12]=3[CH:11]=2)[C:5]([C:19]#[N:20])=[C:4]([O:21][CH2:22][C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[N:3]=1.N(OCCC(C)C)=O.[ClH:37]>C(#N)C.[Cu]Cl>[Cl:37][C:2]1[C:7]([C:8]#[N:9])=[C:6]([C:10]2[CH:18]=[CH:17][C:13]3[O:14][CH2:15][O:16][C:12]=3[CH:11]=2)[C:5]([C:19]#[N:20])=[C:4]([O:21][CH2:22][C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[N:3]=1

Komponenten

6

Edukt 3

HCID 313Hydrochloric AcidHCID 8053Isoamyl NitriteHCID 9799503HCID 9799503, Verbindung

Produkt 1

HCID 17976006HCID 17976006, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 62652Cuprous chlorideKatalysatorHCID 6342AcetonitrileLösungsmittel

Reaktionsbedingungen

Temperatur
40 °C

Versuchsvorschrift

400 mg (1.08 mmol) of 2-amino-4-(1,3-benzodioxol-5-yl)-6-benzyloxy-3,5-pyridinedicarbonitrile (example 1) are dissolved in 10 ml of acetonitrile. 759 mg (0.87 ml, 6.48 mmol) of isoamyl nitrite and 871 mg (6.48 mmol) of copper(I) chloride are then added, and the mixture is stirred at 40° C. for about 16 h. The reaction solution is then diluted with 1N hydrochloric acid and extracted three times with in each case 50 ml of dichloromethane. The combined organic phases are dried with sodium sulfate and concentrated under reduced pressure. The concentration residue is crystallized from dichloromethane/methanol.

Aufarbeitung

  1. extractionextracted three times with in each case 50 ml of dichloromethane
  2. dry with materialThe combined organic phases are dried with sodium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe concentration residue is crystallized from dichloromethane/methanol

Quellen und Nachweise

ORD-Eintrag
ord-6adaf7ac4ba840e48a1c445a12840026
Quelldatensatz
uspto-grants-2010_12
Patentnummer
US07855219B2

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