Potassium Carbonate → Butathiofos

HRID 2296376

Reaktionsgleichung

Reaktionsgleichung von HRID 2296376
[CH3:1][C:2]([C:5]1[N:10]=[CH:9][C:8]([OH:11])=[CH:7][N:6]=1)([CH3:4])[CH3:3].C(=O)([O-])[O-].[K+].[K+].[P:18](=[S:26])(Cl)([O:22][CH2:23][CH3:24])[O:19][CH2:20][CH3:21].[H][H]>C(#N)C>[P:18](=[S:26])([O:11][C:8]1[CH:7]=[N:6][C:5]([C:2]([CH3:1])([CH3:3])[CH3:4])=[N:10][CH:9]=1)([O:22][CH2:23][CH3:24])[O:19][CH2:20][CH3:21]

Komponenten

6

Edukt 4

HCID 11430Potassium CarbonateHCID 17305O,O-diethyl phosphorochloridothioate2×HCID 1634995-Pyrimidinol, 2-(1,1-dimethylethyl)-HCID 178418361HCID 178418361, Verbindung2×

Produkt 1

HCID 185020Butathiofos

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

To a mixture of 98 grams of 2-(1,1-dimethylethyl)-5-pyrimidinol, 130 grams of finely powdered potassium carbonate and 800 ml of acetonitrile was added 121 grams of O,O-diethyl phosphorochloridothioate. The temperature of the reaction mixture rose to 55° C. Stirring was continued until no more starting O,O-diethyl phosphorochloridothioate could be detected by gas-liquid chromatography. The reaction appeared to be complete in about 1 hour. The salts present were then removed by filtration, the filtrate concentrated in a rotary evaporator, the residue taken up in ether, the ether solution washed twice with 2 percent aqueous sodium hydroxide, and once with saturated sodium chloride solution, and dried over anhydrous sodium sulfate. The ether was then removed under vacuum leaving a pale yellow colored oil with a refractive index at 25° of 1.4913. On elemental analysis the product was found to contain by weight 47.38% carbon; 6.67% hydrogen and 9.19% nitrogen. Theoretical analysis is 47.35% carbon; 6.96% hydrogen and 9.21% nitrogen.

Aufarbeitung

  1. customrose to 55° C
  2. customThe salts present were then removed by filtration
  3. concentrationthe filtrate concentrated in a rotary evaporator
  4. washthe ether solution washed twice with 2 percent aqueous sodium hydroxide
  5. dry with materialonce with saturated sodium chloride solution, and dried over anhydrous sodium sulfate
  6. customThe ether was then removed under vacuum
  7. customleaving a pale yellow colored oil with a refractive index at 25° of 1.4913

Quellen und Nachweise

ORD-Eintrag
ord-9e5c469cc0f045e89719d23e887dc714
Quelldatensatz
uspto-grants-1984_01
Patentnummer
US04429125

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