2,4,6-Trichloropyrimidine → HCID 20539467, Verbindung

HRID 224991

Reaktionsgleichung

Reaktionsgleichung von HRID 224991
Cl[C:2]1[N:7]=[C:6](Cl)[CH:5]=[C:4](Cl)[N:3]=1.[C:10]1([P:16]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[O:17]C)[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1>ClC1C=CC=CC=1Cl>[C:10]1([P:16]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)([C:2]2[N:7]=[C:6]([P:16]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)([C:10]3[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=3)=[O:17])[CH:5]=[C:4]([P:16]([C:19]3[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=3)([C:10]3[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=3)=[O:17])[N:3]=2)=[O:17])[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

Komponenten

4

Edukt 2

HCID 773782,4,6-TrichloropyrimidineHCID 77636Methoxydiphenylphosphine

Produkt 1

HCID 20539467HCID 20539467, VerbindungAusbeute 61,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 72391,2-DichlorobenzeneLösungsmittel

Versuchsvorschrift

To a stirred, refluxing mixture of 5.00 g of 2,4,6-trichloropyrimidine in 100 ml of o-dichlorobenzene under nitrogen was added dropwise 26.00 g of methyl diphenylphosphinite. After the addition was completed, the mixture was refluxed for 6.5 hours and then allowed to stand overnight at room temperature. The next day a small amount of the solvent was removed by boiling, and the solution was allowed to stand again overnight. The next day the resulting solid was separated by filtration, washed twice with benzene and three times with hexane, recrystallized from 650 ml of toluene, and dried at 100° C./0.1 mm (13 Pa) to give 11.35 g of 2,4,6-tris(diphenylphosphinyl)pyrimidine (shown by formula in Claim 10) as a white solid, mp 235°-236° C. Anal. Calcd for C40H31N2O3P3 : C, 70.59; H, 4.59; N, 4.12; P, 13.65. Found: C, 70.72; H, 4.90; N, 3.92; P, 13.61.

Aufarbeitung

  1. temperatureTo a stirred, refluxing
  2. additionAfter the addition
  3. temperaturethe mixture was refluxed for 6.5 hours
  4. customThe next day a small amount of the solvent was removed
  5. waitto stand again overnight
  6. customThe next day the resulting solid was separated by filtration
  7. washwashed twice with benzene and three times with hexane
  8. customrecrystallized from 650 ml of toluene
  9. customdried at 100° C./0.1 mm (13 Pa)

Quellen und Nachweise

ORD-Eintrag
ord-f0367442f409431aa76904112d77505f
Quelldatensatz
uspto-grants-1980_11
Patentnummer
US04234729

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