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Triethylamine → HCID 18982007, Verbindung

HRID 1440783
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1440783
[C:1]1([C:7]2[C:12](C(O)=O)=[CH:11][CH:10]=[C:9]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)[N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C1(P(N=[N+]=[N-])(C2C=CC=CC=2)=[O:29])C=CC=CC=1.C([N:41]([CH2:44]C)CC)C.[CH:46]([C:49]1[CH:55]=[CH:54][CH:53]=[C:52]([CH:56]([CH3:58])[CH3:57])[C:50]=1[NH2:51])([CH3:48])[CH3:47]>FC1C=CC=CC=1.O>[CH:56]([C:52]1[CH:53]=[CH:54][CH:55]=[C:49]([CH:46]([CH3:48])[CH3:47])[C:50]=1[NH:51][C:44]([NH:41][C:12]1[C:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)=[N:8][C:9]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)=[CH:10][CH:11]=1)=[O:29])([CH3:58])[CH3:57]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 8471TriethylamineHCID 32484DiisopropylanilineHCID 199401P,P-Diphenylphosphinic azideHCID 18982012HCID 18982012, Verbindung

Produkt 1

HCID 18982007HCID 18982007, VerbindungAusbeute 90,9 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962
Water
Lösungsmittel
HCID 10008FluorobenzeneLösungsmittel

Versuchsvorschrift

To a stirred mixture of 551 mg of 2,6-diphenyl-3-pyridinecarboxylic acid and 0.52 cc of diphenylphosphoryl azide in 6 cc of fluorobenzene was added dropwise 0.29 cc of triethylamine at room temperature. The resulting mixture was stirred at room temperature for 30 minutes and then heated at a temperature of 65°-70° C. for 10 minutes. After cooling, 0.45 cc of 2,6-diisopropylaniline was added and the resulting mixture was heated at a temperature of 70° C. for 1.5 hours. After cooling, water was added to the reaction mixture and extracted with chloroform. The extract was dried over magnesium sulfate, and distilled to remove the solvent. The crude product thus obtained was purified by a silica gel column chromatography (eluent: chloroform) to obtain 817 mg of compound 61.

Aufarbeitung

  1. temperatureheated at a temperature of 65°-70° C. for 10 minutes
  2. temperatureAfter cooling
  3. temperaturethe resulting mixture was heated at a temperature of 70° C. for 1.5 hours
  4. temperatureAfter cooling
  5. extractionextracted with chloroform
  6. dry with materialThe extract was dried over magnesium sulfate
  7. distillationdistilled
  8. customto remove the solvent
  9. customThe crude product thus obtained
  10. customwas purified by a silica gel column chromatography (eluent: chloroform)

Quellen und Nachweise

ORD-Eintrag
ord-f5eca9916cc24f6f9007c595ed1b563b
Quelldatensatz
uspto-grants-1996_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05500424

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