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Triethylamine → HCID 86702333, Verbindung

HRID 2279079
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2279079
C(N(CC)CC)C.Cl[C:9]1[C:14]([N+:15]([O-:17])=[O:16])=[CH:13][CH:12]=[C:11]([Cl:18])[N:10]=1.[Cl:19][C:20]1[CH:21]=[C:22]([NH2:28])[C:23]([O:26][CH3:27])=[N:24][CH:25]=1>C(#N)C>[Cl:18][C:11]1[N:10]=[C:9]([NH:28][C:22]2[C:23]([O:26][CH3:27])=[N:24][CH:25]=[C:20]([Cl:19])[CH:21]=2)[C:14]([N+:15]([O-:17])=[O:16])=[CH:13][CH:12]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 852392,6-Dichloro-3-nitropyridineHCID 451221815-Chloro-2-methoxypyridin-3-amine

Produkt 1

HCID 86702333HCID 86702333, VerbindungAusbeute 39,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Reaktionsbedingungen

Temperatur
90 °C

Versuchsvorschrift

Triethylamine (2.7 mL) and a catalytic amount of 4-diaminopyrimidine were added to a solution of 2,6-dichloro-3-nitropyridine (639 mg, 3.31 mmol) and 5-chloro-2-methoxy pyridin-3-amine (Preparation 23, 501 mg, 3.16 mmol) in acetonitrile (20 mL) and the resulting mixture was stirred overnight at 90° C. Solvent was then removed under reduced pressure until a solid precipitated. The solid was filtered, washed with acetonitrile and dried. The solid was then treated with dichloromethane, filtered, washed with more dichloromethane and the combined filtrate and washings were concentrated to dryness under reduced pressure to yield the title compound (390 mg 30%) as an orange solid.

Aufarbeitung

  1. customSolvent was then removed under reduced pressure until a solid
  2. customprecipitated
  3. filtrationThe solid was filtered
  4. washwashed with acetonitrile
  5. customdried
  6. additionThe solid was then treated with dichloromethane
  7. filtrationfiltered
  8. washwashed with more dichloromethane
  9. concentrationthe combined filtrate and washings were concentrated to dryness under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-f2e83d4dc01c42449d4561a80ba1b238
Quelldatensatz
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09133200B2

Notizen zur Reaktion

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