Pyridine → HCID 59435993, Verbindung

HRID 1802505Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1802505
[Cl:1][C:2]1[CH:3]=[C:4]([C:27](=[N:29][OH:30])[NH2:28])[CH:5]=[C:6]([Cl:26])[C:7]=1[NH:8][C:9]1[C:18]2[CH:19]=[CH:20][N:21]=[C:22]([O:23][CH2:24][CH3:25])[C:17]=2[C:16]2[C:11](=[CH:12][CH:13]=[N:14][CH:15]=2)[N:10]=1.N1C=CC=CC=1.[C:37]([O:40][C:41]([CH3:46])([CH3:45])[C:42](Cl)=O)(=[O:39])[CH3:38]>O1CCOCC1>[C:37]([O:40][C:41]([C:46]1[O:30][N:29]=[C:27]([C:4]2[CH:5]=[C:6]([Cl:26])[C:7]([NH:8][C:9]3[C:18]4[CH:19]=[CH:20][N:21]=[C:22]([O:23][CH2:24][CH3:25])[C:17]=4[C:16]4[C:11](=[CH:12][CH:13]=[N:14][CH:15]=4)[N:10]=3)=[C:2]([Cl:1])[CH:3]=2)[N:28]=1)([CH3:45])[CH3:42])(=[O:39])[CH3:38]

Komponenten

5

Edukt 3

HCID 1049PyridineHCID 1234962-Acetoxyisobutyroyl chlorideHCID 136337086HCID 136337086, Verbindung

Produkt 1

HCID 59435993HCID 59435993, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Reaktionsbedingungen

Temperatur
110 °C

Versuchsvorschrift

To a solution of 3,5-dichloro-4-[(10-ethoxypyrido[4,3-c]-1,6-naphthyridin-6-yl)amino]-N′-hydroxybenzenecarboximidamide (50 mg, 0.11 mmol) in 1,4-dioxane (1 mL) was added pyridine (0.1 mL) and 2-chloro-1,1-dimethyl-2-oxoethyl acetate (0.016 mL, 0.11 mmol). The reaction was heated to 110° C. for 4 h in a sealed tube. After cooling to room temperature, the solvents were evaporated and the residue was dissolved in THF/MeOH, filtered and purified by reverse phase HPLC to afford the title compound.

Aufarbeitung

  1. temperatureAfter cooling to room temperature
  2. customthe solvents were evaporated
  3. dissolutionthe residue was dissolved in THF/MeOH
  4. filtrationfiltered
  5. custompurified by reverse phase HPLC

Quellen und Nachweise

ORD-Eintrag
ord-b5b59a804148446e973be928b4e72a42
Quelldatensatz
uspto-grants-2013_01
Patentnummer
US08349865B2

Notizen zur Reaktion

Wird geladen…