Potassium Carbonate → HCID 86659378, Verbindung

HRID 1187676

Reaktionsgleichung

Reaktionsgleichung von HRID 1187676
[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[C:8]([Cl:10])[N:9]=1)[CH:5]=[O:6].C1(C)C=CC(S([CH2:20][N+:21]#[C-:22])(=O)=O)=CC=1.C(=O)([O-])[O-].[K+].[K+]>CO>[Cl:1][C:2]1[CH:3]=[C:4]([C:5]2[O:6][CH:22]=[N:21][CH:20]=2)[CH:7]=[C:8]([Cl:10])[N:9]=1

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 161915Tosylmethyl isocyanideHCID 27610242,6-Dichloropyridine-4-carbaldehyde

Produkt 1

HCID 86659378HCID 86659378, VerbindungAusbeute 97,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

528 mg of 2,6-dichloroisonicotinaldehyde (this compound was prepared by the method described in J. Chem. Soc., Chem. Commun., 1998, 1567-1568) was dissolved in 10 ml of methanol, and 586 mg of p-toluenesulfonyl methyl isocyanide and 415 mg of potassium carbonate ware added, and the mixture was stirred at 50° C. for 30 minutes. The reaction solution was concentrated, and then diluted with ethyl acetate, and the organic layer was washed with a saturated aqueous solution of sodium bicarbonate and brine, and then dried over magnesium sulfate. The solvent was distilled off under reduced pressure to obtain 630 mg of the objective compound as white powder.

Aufarbeitung

  1. concentrationThe reaction solution was concentrated
  2. additiondiluted with ethyl acetate
  3. washthe organic layer was washed with a saturated aqueous solution of sodium bicarbonate and brine
  4. dry with materialdried over magnesium sulfate
  5. distillationThe solvent was distilled off under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-e49229dca49d4e5b89648b03d2c88c00
Quelldatensatz
uspto-grants-2014_03
Patentnummer
US08673891B2

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