5-Chloro-2-fluoro-4-iodopyridine → HCID 178511614, Verbindung

HRID 1623264Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1623264
[Cl:1][C:2]1[C:3]([I:9])=[CH:4][C:5](F)=[N:6][CH:7]=1.[C@H:10]1([NH2:17])[CH2:15][CH2:14][C@H:13]([NH2:16])[CH2:12][CH2:11]1>CS(C)=O>[Cl:1][C:2]1[C:3]([I:9])=[CH:4][C:5]([NH:16][C@H:13]2[CH2:14][CH2:15][C@H:10]([NH2:17])[CH2:11][CH2:12]2)=[N:6][CH:7]=1

Komponenten

4

Edukt 2

HCID 218653365-Chloro-2-fluoro-4-iodopyridineHCID 178511674HCID 178511674, Verbindung

Produkt 1

HCID 178511614HCID 178511614, VerbindungAusbeute 85,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 679Dimethyl SulfoxideLösungsmittel2×

Reaktionsbedingungen

Temperatur
85 °C

Versuchsvorschrift

A mixture of 5-chloro-2-fluoro-4-iodopyridine (1000 mg, 3.88 mmol), DMSO (7 ml), and trans-cyclohexane-1,4-diamine (2661 mg, 23.31 mmol) reaction mixture was stirred at about 85° C. for 2 hours, followed by LCMS. The crude reaction mixture then was mixed with 5 ml DMSO, filtered and purified by prep LC. After lyapholization, 1.17 grams of the title compound was obtained as a TFA salt. LCMS (m/z): 352.1 (MH+), retention time=0.50 min.

Aufarbeitung

  1. customThe crude reaction mixture
  2. filtrationfiltered
  3. custompurified by prep LC

Quellen und Nachweise

ORD-Eintrag
ord-418e9cc1774e42ad9f4d8e034df7f7a2
Quelldatensatz
uspto-grants-2014_07
Patentnummer
US08778951B2

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