Reaction #5321

Reaction equation

1,1-bis(chlorophenyl)-2,2,2-trichloroethane

dimethylbenzyllaurylammonium chloride

→

1,1-bis(chlorophenyl)-2,2-dichloroethylene

Conditions

Workup

1. 1
   workup.WAITwas continued for 4 hours at 100°
2. 2
   workup.WAITAfter 1 hour at rest
3. 3
   Otherthe aqueous phase was separated off
4. 4
   workup.ADDITION268 kg of 50% strength sodium hydroxide were added
5. 5
   workup.STIRRINGwith stirring at 100° C. for 10 hours
6. 6
   Otherwith 560 kg of water and 1 hour
7. 7
   WashThe organic phase was then washed 3 times with 250 kg of a 1N solution of sulfuric acid

Procedure

990 kg of solid 1,1-bis(chlorophenyl)-2,2,2-trichloroethane were charged into the basic aqueous phase emanating from an upstream dehydrochlorination operation. The charging period was 2 hours to avoid the formation of solid masses inside the reactor. 5 kg of dimethylbenzyllaurylammonium chloride were added, while intense stirring was continued for 4 hours at 100°. After 1 hour at rest, the aqueous phase was separated off and 268 kg of 50% strength sodium hydroxide were added and the dehydrochlorination was continued with stirring at 100° C. for 10 hours. After dilution with 560 kg of water and 1 hour at rest, the organic phase was drawn off and the aqueous phase was retained for the following operation. The organic phase was then washed 3 times with 250 kg of a 1N solution of sulfuric acid and 879 kg of 1,1-bis(chlorophenyl)-2,2-dichloroethylene were obtained.

Source