Reaktion #2726

Reaktionsgleichung

potassium hydroxide

3,4,5,6-tetra-chloro-1,2-dicyanobenzene

phenol

→

3,5,6-Trichloro-1,2-dicyano-4-phenoxybenzene

Lösungsmittel

water

acetone

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   ExtraktionThe aqueous mixture was extracted with dichloromethane (3×500 parts)
2. 2
   WaschenThe dichloromethane extracts were washed with water (3×200 parts)
3. 3
   Trocknendried over anhydrous Na2SO4
4. 4
   Filtrationfiltered
5. 5
   Sonstigethe dichloromethane was removed under reduced pressure
6. 6
   Sonstigeto leave a brown solid
7. 7
   SonstigeThe solid was recrystallised from butan-1-ol

Vorschrift

A solution of potassium hydroxide (11.2 parts) in water (22 parts) was added dropwise to a stirred solution of 3,4,5,6-tetra-chloro-1,2-dicyanobenzene (26.6 parts) and phenol (9.4 parts) in acetone (100 arts) at 0° C. The solution was stirred at 60° C. for 2 hours before pouring into water (500 parts). The aqueous mixture was extracted with dichloromethane (3×500 parts). The dichloromethane extracts were washed with water (3×200 parts), dried over anhydrous Na2SO4, filtered and the dichloromethane was removed under reduced pressure to leave a brown solid. The solid was recrystallised from butan-1-ol. 3,5,6-Trichloro-1,2-dicyano-4-phenoxybenzene (17 parts) was obtained as a brown solid, m.p. 147°-150° C.

Quelle