Potassium Carbonate → HCID 13277769, Verbindung

HRID 2296379Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2296379
[CH2:1]([C:3]1[N:8]=[CH:7][C:6]([OH:9])=[CH:5][N:4]=1)[CH3:2].C(=O)([O-])[O-].[K+].[K+].[P:16]([S:22][CH2:23][CH:24]([CH3:26])[CH3:25])(=[S:21])(Cl)[O:17][CH2:18][CH3:19].[H][H]>C(#N)C>[P:16]([S:22][CH2:23][CH:24]([CH3:26])[CH3:25])(=[S:21])([O:9][C:6]1[CH:5]=[N:4][C:3]([CH2:1][CH3:2])=[N:8][CH:7]=1)[O:17][CH2:18][CH3:19]

Komponenten

6

Edukt 4

HCID 11430Potassium CarbonateHCID 13079909O-Ethyl S-(2-methylpropyl) phosphorochloridodithioateHCID 136077292-Ethylpyrimidin-5-olHCID 178418361HCID 178418361, Verbindung2×

Produkt 1

HCID 13277769HCID 13277769, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

A mixture of 5 grams of 2-ethyl-5-pyrimidinol, 5 grams of finely powdered potassium carbonate, 40 ml of acetonitrile and 9.3 grams of O-ethyl S-(2-methylpropyl) phosphorochloridodithioate was stirred without external heating overnight. The solids were then removed by filtration, the filtrate concentrated under vacuum, the residue taken up in diethyl ether, the ether solution washed twice with 2% aqueous sodium hydroxide, once with saturated sodium chloride solution and dried over anhydrous sodium sulfate. The solvent was removed in a rotary evaporator leaving a pale amber colored oil having a refractive index of 25° of 1.5296. Elemental analysis showed the product contained 44.81% carbon; 6.58% hydrogen and 8.59% nitrogen. Theoretical analysis is 44.98% carbon; 6.61% hydrogen and 8.74% nitrogen.

Aufarbeitung

  1. temperaturewithout external heating overnight
  2. customThe solids were then removed by filtration
  3. concentrationthe filtrate concentrated under vacuum
  4. washthe ether solution washed twice with 2% aqueous sodium hydroxide, once with saturated sodium chloride solution
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe solvent was removed in a rotary evaporator
  7. customleaving a pale amber

Quellen und Nachweise

ORD-Eintrag
ord-49307633203d45e9ab4f72387e95691e
Quelldatensatz
uspto-grants-1984_01
Patentnummer
US04429125

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