تفاعل #1809103

ord-9c556aed82b242fd9db6bc1713745798

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.DISSOLUTIONare dissolved in 100 ml of abs
  2. 2
    غسيلThe reaction mixture is then washed with 2×100 ml of water
  3. 3
    تجفيفdried over sodium sulfate
  4. 4
    ترشيحfiltered
  5. 5
    أخرىThe solvent is removed by evaporation
  6. 6
    workup.DISTILLATIONthe oily residue is purified by high vacuum distillation

الإجراء التجريبي

12.7 parts of the 2-(4'-chloro-2'-difluoromethoxyphenyl)-2-methyl-4-ethyl-1,3-dioxolane prepared in (a) are dissolved in 100 ml of abs. chloroform and the solution is warmed to 30° C. Under irradiation with a 150 watt spot lamp, 7.3 parts of bromine in 30 ml of abs. chloroform are added dropwise over 1 hour and the reaction mixture is then stirred for 2 hours at room temperature. The reaction mixture is then washed with 2×100 ml of water, dried over sodium sulfate, and filtered. The solvent is removed by evaporation and the oily residue is purified by high vacuum distillation; b.p. 113°-115° C./0.05 mbar.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04853399uspto-grants-1989_08