반응 #213864

ord-92d69f50b91f450fb5744ced5dbdbe85

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was warmed to 40°
  2. 2
    온도maintaining a reaction temperature of about 40°
  3. 3
    세척after which it was washed with an aqueous solution
  4. 4
    workup.ADDITIONcontaining 20% sodium carbonate
  5. 5
    기타The organic phase was separated from the mixture
  6. 6
    기타the solvent removed by distillation under reduced pressure

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04254051uspto-grants-1981_03