تفاعل #5321

ord-e272024058c04429a4fb231ad4f05a1a

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.WAITwas continued for 4 hours at 100°
  2. 2
    workup.WAITAfter 1 hour at rest
  3. 3
    أخرىthe 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
    أخرىwith 560 kg of water and 1 hour
  7. 7
    غسيلThe organic phase was then washed 3 times with 250 kg of a 1N solution of sulfuric acid

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05243110uspto-grants-1993_09