Hexane → HCID 12092217, Verbindung

HRID 224989

Reaktionsgleichung

Reaktionsgleichung von HRID 224989
Cl[C:2]1[C:11](Cl)=[N:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[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.[CH3:28][CH2:29][CH2:30][CH2:31][CH2:32][CH3:33]>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]([P:19]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)([C:30]3[CH:29]=[CH:28][CH:33]=[CH:32][CH:31]=3)=[O:20])=[N:10][C:9]3[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=3)[N:3]=2)=[O:20])[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

Komponenten

5

Edukt 3

HCID 8058HexaneHCID 166592,3-DichloroquinoxalineHCID 77636Methoxydiphenylphosphine

Produkt 1

HCID 12092217HCID 12092217, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 72391,2-DichlorobenzeneLösungsmittel

Versuchsvorschrift

To a stirred, refluxing mixture of 5.00 g of 2,3-dichloroquinoxaline in 100 ml of o-dichlorobenzene under nitrogen was added dropwise 14.00 g of methyl diphenylphosphinite. The mixture was refluxed for 6 hours after the addition was completed and then allowed to stand overnight at room temperature. The next day the mixture was admixed with 500 ml of n-hexane, and the resulting solid was separated by filtration, washed with hexane, recrystallized from 100 ml of chlorobenzene, and dried at 100° C./0.1 mm (13 Pa) to give 9.87 g of 2,3-bis(diphenylphosphinyl)-quinoxaline (shown by formula in Claim 6) as a very slightly yellowish-white solid, mp 258°-272° C. with decomposition. Anal. Calcd for C32H24N2O2P2 : C, 72.45; H, 4.56; N, 5.28; P, 11.68. Found: C, 72.38; H, 4.23; N, 5.18; P, 11.39.

Aufarbeitung

  1. temperatureTo a stirred, refluxing
  2. temperatureThe mixture was refluxed for 6 hours
  3. additionafter the addition
  4. customthe resulting solid was separated by filtration
  5. washwashed with hexane
  6. customrecrystallized from 100 ml of chlorobenzene
  7. customdried at 100° C./0.1 mm (13 Pa)

Quellen und Nachweise

ORD-Eintrag
ord-4a8166e94d6b4475a4cff1db11e3f1d1
Quelldatensatz
uspto-grants-1980_11
Patentnummer
US04234729

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