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Triethylamine → HCID 22637131, Verbindung

HRID 2416023
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2416023
[Cl:1][C:2]1[CH:3]=[C:4]([CH:6]=[CH:7][C:8]=1[O:9][C:10]1[C:19]2[C:14](=[CH:15][C:16]([O:22][CH3:23])=[C:17]([O:20][CH3:21])[CH:18]=2)[N:13]=[CH:12][N:11]=1)[NH2:5].C(N(CC)CC)C.Cl[C:32](Cl)([O:34]C(=O)OC(Cl)(Cl)Cl)Cl.[NH2:43][C:44]1[O:48][N:47]=[C:46]([CH3:49])[CH:45]=1>C(Cl)(Cl)Cl.O>[Cl:1][C:2]1[CH:3]=[C:4]([NH:5][C:32]([NH:43][C:44]2[O:48][N:47]=[C:46]([CH3:49])[CH:45]=2)=[O:34])[CH:6]=[CH:7][C:8]=1[O:9][C:10]1[C:19]2[C:14](=[CH:15][C:16]([O:22][CH3:23])=[C:17]([O:20][CH3:21])[CH:18]=2)[N:13]=[CH:12][N:11]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 8471TriethylamineHCID 845905-Amino-3-methylisoxazoleHCID 94429TriphosgeneHCID 218905643-Chloro-4-[(6,7-dimethoxy-4-quinazolinyl)oxy]aniline

Produkt 1

HCID 22637131HCID 22637131, VerbindungAusbeute 58,6 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962
Water
Lösungsmittel
HCID 6212ChloroformLösungsmittel2×

Versuchsvorschrift

3-Chloro-4-[(6,7-dimethoxy-4-quinazolinyl)oxy]-aniline (84 mg) was dissolved in chloroform (2.5 ml) and triethylamine (0.25 ml) to prepare a solution. A solution of triphosgene (38 mg) in chloroform was then added to the solution, and the mixture was stirred at room temperature for 5 min. Next, 5-amino-3-methylisoxazole (27 mg) was added thereto, and the mixture was further stirred at room temperature overnight. Water was added to the reaction solution, and the mixture was subjected to separatory extraction with chloroform. The organic layer was concentrated and was evaporated to dryness. Diethyl ether was added to the resultant solid, and the solid was collected by filtration and was further washed with methyl alcohol to give the title compound (34.2 mg, yield 30%).

Aufarbeitung

  1. stirringthe mixture was further stirred at room temperature overnight
  2. extractionthe mixture was subjected to separatory extraction with chloroform
  3. concentrationThe organic layer was concentrated
  4. customwas evaporated to dryness
  5. additionDiethyl ether was added to the resultant solid
  6. filtrationthe solid was collected by filtration
  7. washwas further washed with methyl alcohol

Quellen und Nachweise

ORD-Eintrag
ord-6291a111ab544c3f88404cd7c2207603
Quelldatensatz
uspto-grants-2004_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06821987B2

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