4,6-Dichloro-2-(methylthio)pyrimidine → HCID 20539481, Verbindung

HRID 1065630Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1065630
[CH:1]1([P:7]([CH:10]2[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]2)[O:8]C)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.Cl[C:17]1[CH:22]=[C:21](Cl)[N:20]=[C:19]([S:24][CH3:25])[N:18]=1>ClC1C=CC=CC=1Cl>[CH:1]1([P:7]([CH:10]2[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]2)([C:17]2[CH:22]=[C:21]([P:7]([CH:10]3[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15]3)([CH:1]3[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]3)=[O:8])[N:20]=[C:19]([S:24][CH3:25])[N:18]=2)=[O:8])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

Komponenten

4

Edukt 2

HCID 805314,6-Dichloro-2-(methylthio)pyrimidineHCID 6931439Phosphinous acid, dicyclohexyl-, methyl ester

Produkt 1

HCID 20539481HCID 20539481, VerbindungAusbeute 5,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 72391,2-DichlorobenzeneLösungsmittel

Versuchsvorschrift

A mixture of 2.50 g of methyl dicyclohexylphosphinite and 1.00 g of 4,6-dichloro-2-methylthiopyrimidine in 20 ml of o-dichlorobenzene was refluxed under nitrogen for 6.5 hours. Volatiles were removed from the mixture under vacuum, and the resulting oily residue was recrystallized twice from cyclohexane with decolorizing charcoal treatment and dried at 100° C./0.1 mm (13 Pa) to give 0.15 g of 4,6-bis(dicyclohexylphosphinyl)-2-methylthiopyrimidine as white crystals, mp 197°-198.5° C. Anal. Calcd for C29H48N2O2P2S: C, 63.25; H, 8.79; N, 5.07; S, 5.82. Found: C, 63.19; H, 8.81; N, 4.89; S, 6.04.

Aufarbeitung

  1. temperaturewas refluxed under nitrogen for 6.5 hours
  2. customVolatiles were removed from the mixture under vacuum
  3. customthe resulting oily residue was recrystallized twice from cyclohexane with decolorizing charcoal treatment
  4. customdried at 100° C./0.1 mm (13 Pa)

Quellen und Nachweise

ORD-Eintrag
ord-704f4a33043543b18857934e58b7b5f5
Quelldatensatz
uspto-grants-1982_05
Patentnummer
US04330461

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