تفاعل #213864

ord-92d69f50b91f450fb5744ced5dbdbe85

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas warmed to 40°
  2. 2
    درجة الحرارةmaintaining a reaction temperature of about 40°
  3. 3
    غسيلafter which it was washed with an aqueous solution
  4. 4
    workup.ADDITIONcontaining 20% sodium carbonate
  5. 5
    أخرىThe organic phase was separated from the mixture
  6. 6
    أخرىthe solvent removed by distillation under reduced pressure

الإجراء التجريبي

A stirred mixture of sodium cyanide (18.0 g, 0.36 mole) and 3-(cyclohexylamino)propanesulfonic acid (1.34 g, 0.006 mole) in 300 ml of water was warmed to 40°. During a one hour period, maintaining a reaction temperature of about 40°, a solution of cis-3-(2,2-dichloroethenyl)-2,2-dimethylcyclopropanecarbonyl chloride (71.7 g, 0.315 mole) and 3-phenoxybenzaldehyde (61.9 g, 0.3 mole) in 262.2 g of n-heptane was added. The mixture was then stirred at 40° for one additional hour, after which it was washed with an aqueous solution containing 20% sodium carbonate and then with water. The organic phase was separated from the mixture and the solvent removed by distillation under reduced pressure to give α-cyano-3-phenoxybenzyl cis-3-(2,2-dichloroethenyl)-2,2-dimethylcyclopropanecarboxylate.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04254051uspto-grants-1981_03