Reaktion #363324

Reaktionsgleichung

phosgene

phosgene

benzaldehyde cyanohydrin

phosgene

N2

→

α-chlorophenylacetonitrile

Lösungsmittel

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturheated
2. 2
   SonstigeAt 99° C.
3. 3
   Sonstigeare gassed in over the course of 10 minutes
4. 4
   TemperaturThe internal temperature is maintained between 99 and 102° C. throughout
5. 5
   SonstigeAfter a post-reaction of 60 minutes at 99° C.
6. 6
   Sonstigeat 50° C.
7. 7
   Sonstigefor 2.5 h
8. 8
   workup.DISTILLATIONThe discharge of 359 g is fractionally distilled on a 30 cm Vigreux column
9. 9
   Sonstigeof from 68 to 73° C

Vorschrift

150 g of toluene and 7 g (0.02 mol) of Cyanex® 923 are initially introduced into a phosgenation apparatus with attached carbonic acid condenser and heated. At 99° C., 13 g of phosgene are gassed in over the course of 10 minutes. Thereafter, over the course of 2 hours, 192 g (1.44 mol) of benzaldehyde cyanohydrin and a further 149 g (total=172 g or 1.74 mol) of phosgene are added in parallel. The internal temperature is maintained between 99 and 102° C. throughout. After a post-reaction of 60 minutes at 99° C., excess phosgene is stripped out using N2 at 50° C. for 2.5 h. The discharge of 359 g is fractionally distilled on a 30 cm Vigreux column. The main fraction passes over at 0.6 mbar and a head temperature of from 68 to 73° C. 192.7 g (88.3% of theory) of α-chlorophenylacetonitrile are isolated.

Quelle