Hydrochloric Acid → Ethyl 2-isopropoxy-4-methoxybenzimidate hydrochloride

HRID 1167304Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1167304
[ClH:1].[CH:2]([O:5][C:6]1[CH:13]=[C:12]([O:14][CH3:15])[CH:11]=[CH:10][C:7]=1[C:8]#[N:9])([CH3:4])[CH3:3].[CH2:16]([OH:18])[CH3:17]>>[ClH:1].[CH:2]([O:5][C:6]1[CH:13]=[C:12]([O:14][CH3:15])[CH:11]=[CH:10][C:7]=1[C:8](=[NH:9])[O:18][CH2:16][CH3:17])([CH3:4])[CH3:3]

Komponenten

4

Edukt 3

HCID 313Hydrochloric Acid2×HCID 702EthanolHCID 227210812-Isopropoxy-4-methoxybenzonitrile

Produkt 1

HCID 21896893Ethyl 2-isopropoxy-4-methoxybenzimidate hydrochlorideAusbeute 99 %

Reaktionsbedingungen

Temperatur
-10 °C

Versuchsvorschrift

Hydrogen chloride gas was passed through a solution of 2-isopropoxy-4-methoxy-benzonitrile (11.5 g, 60.14 mmol) in anhydrous ethanol (250 mL) cooled to −10° C. After 45 min, hydrogen chloride gas was stopped and the reaction mixture was stirred at room temperature in a closed reaction vessel for 2 weeks. The reaction vessel was cooled to 0° C. before the stopper was removed. Argon gas was passed through the solution to remove excess hydrogen chloride gas. The solvent was evaporated and the residue was triturated in diethyl ether (100 mL) to afford ethyl 2-isopropoxy-4-methoxy-benzimidate hydrochloride (16.3 g, 99%). It was used without further purification.

Aufarbeitung

  1. temperatureThe reaction vessel was cooled to 0° C. before the stopper
  2. customwas removed
  3. customto remove excess hydrogen chloride gas
  4. customThe solvent was evaporated
  5. customthe residue was triturated in diethyl ether (100 mL)

Quellen und Nachweise

ORD-Eintrag
ord-569752e827a34fd0a523bb50db91fa0e
Quelldatensatz
uspto-grants-2003_09
Patentnummer
US06617346B1

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