Phosphorus pentachloride → 8,11-Dichlorodibenzo[b,f][1,4]oxazepine

HRID 355672

Reaktionsgleichung

Reaktionsgleichung von HRID 355672
[Cl:1][C:2]1[CH:17]=[CH:16][C:5]2[O:6][C:7]3[CH:15]=[CH:14][CH:13]=[CH:12][C:8]=3[C:9](=O)[NH:10][C:4]=2[CH:3]=1.P(Cl)(Cl)(Cl)(Cl)[Cl:19]>C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:17]=[CH:16][C:5]2[O:6][C:7]3[CH:15]=[CH:14][CH:13]=[CH:12][C:8]=3[C:9]([Cl:19])=[N:10][C:4]=2[CH:3]=1

Komponenten

4

Edukt 2

HCID 24819Phosphorus pentachlorideHCID 766192-Chlorodibenz(b,f)-1,4-oxazepin-11(10H)-one

Produkt 1

HCID 189404158,11-Dichlorodibenzo[b,f][1,4]oxazepineAusbeute 89,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

To a stirred solution of 8-chloro-10,11-dihydrodibenz[b,f][1,4]oxazepin-11-one (0.53 g, 2.15 mmol) in toluene (20 mL) was added phosphorus pentachloride (0.54 g, 2.58 mmol) at room temperature under argon. The resulting mixture was heated at reflux for 4 h and the solvent was removed in vacuo. The residue was redissolved in toluene and reconcentrated. The light yellow solid 8,11-dichlorodibenz[b,f][1,4]oxazepine (0.51 g, quantitative yield) was used directly for the next reaction without further purification.

Aufarbeitung

  1. temperatureThe resulting mixture was heated
  2. temperatureat reflux for 4 h
  3. customthe solvent was removed in vacuo
  4. dissolutionThe residue was redissolved in toluene

Quellen und Nachweise

ORD-Eintrag
ord-4a7b70353d994fcf846d7799bc15809e
Quelldatensatz
uspto-grants-1998_11
Patentnummer
US05834459

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