Hexane → HCID 20539488, Verbindung

HRID 224995

Reaktionsgleichung

Reaktionsgleichung von HRID 224995
Cl[C:2]1[N:3]=[N:4][C:5](Cl)=[CH:6][CH:7]=1.[C:9]1([P:15]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[O:16]C)[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.[CH3:24][CH2:25][CH2:26][CH2:27][CH2:28][CH3:29]>ClC1C=CC=CC=1Cl>[C:9]1([P:15]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)([C:2]2[N:3]=[N:4][C:5]([P:15]([C:9]3[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=3)([C:26]3[CH:25]=[CH:24][CH:29]=[CH:28][CH:27]=3)=[O:16])=[CH:6][CH:7]=2)=[O:16])[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1

Komponenten

5

Edukt 3

HCID 8058HexaneHCID 673313,6-DichloropyridazineHCID 77636Methoxydiphenylphosphine

Produkt 1

HCID 20539488HCID 20539488, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 72391,2-DichlorobenzeneLösungsmittel

Versuchsvorschrift

To a stirred, refluxing solutionof 3.00 g of 3,6-dichloropyridazine in 50 ml of o-dichlorobenzene under nitrogen was added dropwise 10.00 g of methyl diphenylphosphinite. After the addition was completed, the mixture was refluxed for 7 hours and then cooled. The cooled mixture was mixed with excess hexane; the oil which formed slowly crystallized. The resultant solid was separated by filtration, washed with hexane, and recrystallized twice from ethanol with decolorizing charcoal treatment to give 0.93 g of 3,6-bis-(diphenylphosphinyl)pyridazine (shown by formula in Claim 14) as slightly off-white crystals, mp 248°-251.5° C. Anal. Calcd for C28H22N2O2P2 : C, 70.00; H, 4.62; N, 5.83; P, 12.89. Found: C, 69.72; H, 4.92; N, 5.78; P, 12.82.

Aufarbeitung

  1. additionAfter the addition
  2. temperaturethe mixture was refluxed for 7 hours
  3. temperaturecooled
  4. customthe oil which formed slowly
  5. customcrystallized
  6. customThe resultant solid was separated by filtration
  7. washwashed with hexane
  8. customrecrystallized twice from ethanol with decolorizing charcoal treatment

Quellen und Nachweise

ORD-Eintrag
ord-280ff5bb507745b8a324e341cf0b8fe7
Quelldatensatz
uspto-grants-1980_11
Patentnummer
US04234729

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