Reaktion #6168

Reaktionsgleichung

hydrogen chloride

Ethanol

hydrogen chloride

4-[5-(2-methoxyphenoxy)pentoxy]benzonitrile

→

ethyl 4-[5-(2-methoxyphenoxy)pentoxy]benzenecarboximidate hydrochloride

Lösungsmittel

diethyl ether

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstige(~8 hours)
2. 2
   Sonstigeis 5° C
3. 3
   Temperaturthe temperature range maintained
4. 4
   Sonstigeis 5°-10° C
5. 5
   Sonstigeprecipitation
6. 6
   workup.STIRRINGThe slurry is stirred for 1 hours
7. 7
   Filtrationfiltered
8. 8
   WaschenThe filter cake is washed with diethyl ether (3×4 L)
9. 9
   Sonstigeair-dried for 1/2 hour

Vorschrift

Ethanol (2 B anhydrous, 16.5 L) is cooled with an ice-salt bath to 0° C. Anhydrous hydrogen chloride is introduced until the solution is saturated (~8 hours). At this time the internal temperature is 5° C. To this is added 4-[5-(2-methoxyphenoxy)pentoxy]benzonitrile (1.64 kg, 5.26 mol) as a solid within a period of 10 minutes. At this point additional hydrogen chloride is introduced to maintain saturation at 5° C. for another 8 hours. Almost complete solution is achieved and the color is yellow. The reaction mixture is stirred for a total of 84 hours and the temperature range maintained is 5°-10° C. The resulting slurry is diluted with diethyl ether (52 L) to complete precipitation. The slurry is stirred for 1 hours and filtered. The filter cake is washed with diethyl ether (3×4 L) and air-dried for 1/2 hour to yield ethyl 4-[5-(2-methoxyphenoxy)pentoxy]benzenecarboximidate hydrochloride which is used directly in the next step.

Quelle