تفاعل #215404

ord-992cbbc8a9db43cab0509ab776a9b49f

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىReaction temperature
  2. 2
    درجة الحرارةincreases from 24° to 44° C
  3. 3
    workup.STIRRINGAfter stirring for an additional 1/2 hour
  4. 4
    أخرىreaction mixture
  5. 5
    استخلاصextracted with hexane
  6. 6
    غسيلThe combined hexane extracts are washed with water
  7. 7
    تجفيفdried over MgSO4
  8. 8
    أخرىSolvent is evaporated

الإجراء التجريبي

Into a three-necked 300 ml round-bottom flask are charged 7.4 g (0.15 mole) of sodium cyanide and 80 ml of dimethyl sulfoxide. To this slurry is added 30 g (0.13 mole) of 2-phenoxybenzyl chloride dropwise. Reaction temperature increases from 24° to 44° C. The reaction mixture is stirred for an additional 11/2 hours. To this reaction mixture is added 13.7 g (0.13 mole) of butyl chloride followed by dropwise addition of 34 g (0.4 mole) of 50% sodium hydroxide solution. After stirring for an additional 1/2 hour, reaction mixture is poured into 150 ml of water and extracted with hexane. The combined hexane extracts are washed with water and dried over MgSO4. Solvent is evaporated to give 32 g of crude product. Material can be further purified by vacuum distillation (bp 149-60/0.25 mm).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04259339uspto-grants-1981_03