Phosphorus oxychloride → HCID 17780353, Verbindung

HRID 2187659Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2187659
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[NH:9][C:10]3[C:15]([CH:16]=2)=[CH:14][C:13]([O:17][C:18]([F:21])([F:20])[F:19])=[CH:12][CH:11]=3)=[CH:4][CH:3]=1.C([N:25]1[CH2:29][C:28](=O)[N:27]=[CH:26]1)(=O)C.P(Cl)(Cl)([Cl:33])=O>>[ClH:33].[NH:27]1[CH2:28][CH2:29][N:25]=[C:26]1[C:16]1[C:15]2[C:10](=[CH:11][CH:12]=[C:13]([O:17][C:18]([F:21])([F:19])[F:20])[CH:14]=2)[NH:9][C:8]=1[C:5]1[CH:4]=[CH:3][C:2]([CH3:1])=[CH:7][CH:6]=1

Komponenten

4

Edukt 3

HCID 24813Phosphorus oxychlorideHCID 18476298HCID 18476298, VerbindungHCID 22350258N-acetyl-2-imidazolinone

Produkt 1

HCID 17780353HCID 17780353, Verbindung

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

380 mg (1.3 mmol) of the indole from Step A was heated with 210 mg (1.6 mmol) of N-acetyl-2-imidazolinone in 1.3 ml of neat phosphoryl chloride at 60° C. for 20 h. The excess of phosphoryl chloride was removed under reduced pressure, and the residue was dissolved in 2 ml of absolute ethanol and heated at 60° C. for 5 h. The mixture was cooled, and the crystalline precipitate collected by filtration, washed with ethanol, and dried in vacuo.

Aufarbeitung

  1. customThe excess of phosphoryl chloride was removed under reduced pressure
  2. dissolutionthe residue was dissolved in 2 ml of absolute ethanol
  3. temperatureThe mixture was cooled
  4. filtrationthe crystalline precipitate collected by filtration
  5. washwashed with ethanol
  6. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-84807a0a3561482eb676cd05de1762a2
Quelldatensatz
uspto-grants-2002_06
Patentnummer
US06410562B1

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