تفاعل #5320

ord-14dbf4ab6e104d8e99acc3f339bbd870

ظروف التفاعل

درجة الحرارة
93°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe temperature increased from 93° to 103° C
  2. 2
    درجة الحرارةthe temperature was maintained between 100° and 105° C. for 14 hours, 30 min
  3. 3
    أخرىThe organic phase was separated off by phase separation
  4. 4
    غسيلwashed three times with 100 g of a 1N solution of sulfuric acid

الإجراء التجريبي

150 g of solid 1,1-bis(chlorophenyl)-2,2,2-trichloroethane were added to 248.8 g of a 27.2% strength aqueous sodium hydroxide solution maintained at 93° C. 1.4 g of dimethyllaurylbenzylammonium chloride were added thereto. The temperature increased from 93° to 103° C. The addition of solid 1,1-bis(chlorophenyl)-2,2,2-trichloroethane was continued up to a total amount of 300 g. 1.1 g of dimethyllaurylbenzylammonium chloride were added again and the temperature was maintained between 100° and 105° C. for 14 hours, 30 min. The organic phase was separated off by phase separation and washed three times with 100 g of a 1N solution of sulfuric acid and with water (100 g). 263.7 g of 1,1-bis(chlorophenyl)-2,2-dichloroethylene were obtained (y=98.0%) with 0.09% of 1,1-bis(chlorophenyl)-2,2,2-trichloroethane.

المصدر

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