Phosphorus oxychloride → HCID 13345862, Verbindung

HRID 745661

Reaktionsgleichung

Reaktionsgleichung von HRID 745661
[NH2:1][C:2]1[CH:15]=[C:14]2[C:16]3[C:17]4[C:11]([C:12](=[O:18])[O:13]2)=[CH:10][C:9]([NH2:19])=[CH:8][C:7]=4[O:6][C:5](=[O:20])[C:4]=3[CH:3]=1.P(Cl)(Cl)(Cl)=O.[CH:26]([N:28]1[CH2:32][CH2:31][CH2:30][CH2:29]1)=O.C(Cl)(Cl)Cl.CO>O1CCCC1>[N:28]1([CH:26]=[N:19][C:9]2[CH:8]=[C:7]3[C:17]4[C:16]5[C:4]([C:5](=[O:20])[O:6]3)=[CH:3][C:2]([N:1]=[CH:26][N:28]3[CH2:32][CH2:31][CH2:30][CH2:29]3)=[CH:15][C:14]=5[O:13][C:12](=[O:18])[C:11]=4[CH:10]=2)[CH2:32][CH2:31][CH2:30][CH2:29]1

Komponenten

6

Edukt 4

HCID 24813Phosphorus oxychlorideHCID 773721-PyrrolidinecarboxaldehydeHCID 125070622,7-Diamino-5,10-dioxo-4,5,9,10-tetrahydro-4,9-dioxapyreneHCID 21584188Chloroform methanol

Produkt 1

HCID 13345862HCID 13345862, VerbindungAusbeute 68 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

A suspension of 2,7-diamino-5,10-dioxo-4,5,9,10-tetrahydro-4,9-dioxapyrene (500 mg) in tetrahyrofuran (4 ml) was added to a mixture of phosphorus oxychloride (0.7 ml) and N-formylpyrrolidine (2 ml) and tetrahydrofuran (4 ml), the temperature of the mixture being kept at 5° C. The resulting mixture was stirred for 30 minutes at room temperature, heated at 80° C. for 1 hour and worked up as described in Example 1, paragraph 1. Yield 68%, melting point 275° C. (decomposition) (CHCl3 /methanol).

Aufarbeitung

  1. custombeing kept at 5° C
  2. temperatureheated at 80° C. for 1 hour

Quellen und Nachweise

ORD-Eintrag
ord-7bcbf0c91f254bc3b16ead79e10d1623
Quelldatensatz
uspto-grants-1986_07
Patentnummer
US04599409

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