Hexane → HCID 20539492, Verbindung

HRID 224988

Reaktionsgleichung

Reaktionsgleichung von HRID 224988
Cl[C:2]1[CH:7]=[C:6](Cl)[N:5]=[C:4]([S:9][CH3:10])[N:3]=1.[C:11]1([P:17]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[O:18]C)[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.[CH3:26][CH2:27][CH2:28][CH2:29][CH2:30][CH3:31]>ClC1C=CC=CC=1Cl>[C:11]1([P:17]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)([C:2]2[CH:7]=[C:6]([P:17]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)([C:28]3[CH:27]=[CH:26][CH:31]=[CH:30][CH:29]=3)=[O:18])[N:5]=[C:4]([S:9][CH3:10])[N:3]=2)=[O:18])[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1

Komponenten

5

Edukt 3

HCID 8058HexaneHCID 77636MethoxydiphenylphosphineHCID 805314,6-Dichloro-2-(methylthio)pyrimidine

Produkt 1

HCID 20539492HCID 20539492, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 72391,2-DichlorobenzeneLösungsmittel

Versuchsvorschrift

To a stirred refluxing solution of 5.00 g of 4,6-dichloro-2-methylthiopyrimidine in 150 ml of o-dichlorobenzene under nitrogen was added dropwise 15.00 g of methyl diphenylphosphinite over 35 minutes. The mixture was refluxed for 5.5 hours after the addition was completed and then allowed to cool, at which time it was added to 850 ml of n-hexane. The resulting solid was separated by filtration, washed with n-hexane, and recrystallized from 100 ml of ethanol to give 11.00 g of 4,6-bis(diphenylphosphinyl)-2-methylthiopyrimidine (shown by formula in Claim 8) as white crystals, mp 221°-222° C. Anal. Calcd for C29H24N2O2P2S: C, 66.15; H, 4.59; N, 5.32. Found: C, 65.59; 65.59; H, 4.54, 4.75; N, 5.04, 5.01.

Aufarbeitung

  1. temperatureThe mixture was refluxed for 5.5 hours
  2. additionafter the addition
  3. temperatureto cool, at which time it
  4. customThe resulting solid was separated by filtration
  5. washwashed with n-hexane
  6. customrecrystallized from 100 ml of ethanol

Quellen und Nachweise

ORD-Eintrag
ord-dd40434377704e66bcdb9580ce352c92
Quelldatensatz
uspto-grants-1980_11
Patentnummer
US04234729

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