Methoxydiphenylphosphine → 1,4-Bis(diphenylphosphinyl)phthalazine

HRID 1065629Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1065629
Cl[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5](Cl)=[N:4][N:3]=1.[C:13]1([P:19]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[O:20]C)[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>ClC1C=CC=CC=1Cl>[C:13]1([P:19]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)([C:2]2[C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]([P:19]([C:22]3[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=3)([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)=[O:20])=[N:4][N:3]=2)=[O:20])[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

Komponenten

4

Edukt 2

HCID 77636MethoxydiphenylphosphineHCID 784901,4-Dichlorophthalazine

Produkt 1

HCID 205394661,4-Bis(diphenylphosphinyl)phthalazineAusbeute 48,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 72391,2-DichlorobenzeneLösungsmittel

Versuchsvorschrift

To a stirred, refluxing mixture of 5.00 g of 1,4-dichlorophthalazine in 50 ml of o-dichlorobenzene under nitrogen was added dropwise 15.00 g of methyl diphenylphosphinite. After the addition was completed, the mixture was refluxed for 6 hours and then allowed to stand at room temperature for 13 days. The resulting solid was separated by filtration, washed with benzene and with hexane, recrystallized from 125 ml of toluene with decolorizing charcoal treatment, and dried at 100° C./0.1 mm (13 Pa) to give 6.41 g of 1,4-bis(diphenylphosphinyl)phthalazine (shown by formula in claim 6) as a light-yellow solid, mp 225°-228.5° C. Anal. Calcd for C32H24N2O2P2 : C, 72.45; H, 4.56; N, 5.28; P, 11.68. Found: C, 72.49; H, 4.62; N, 5.36; P, 11.95.

Aufarbeitung

  1. temperatureTo a stirred, refluxing
  2. additionAfter the addition
  3. temperaturethe mixture was refluxed for 6 hours
  4. customThe resulting solid was separated by filtration
  5. washwashed with benzene and with hexane
  6. customrecrystallized from 125 ml of toluene with decolorizing charcoal treatment
  7. customdried at 100° C./0.1 mm (13 Pa)

Quellen und Nachweise

ORD-Eintrag
ord-d44c1073c2344b6294e505bf32a168ee
Quelldatensatz
uspto-grants-1982_05
Patentnummer
US04330461

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