تفاعل #95402

ord-bc78c4a0c5b148f591dbeb66b6a477aa

المذيبات

ظروف التفاعل

درجة الحرارة
25°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    ترشيحthe reaction mixture is filtered
  2. 2
    غسيلthe filtrate is successively washed with 2 N sodium bicarbonate solution, 2 N hydrochloric acid and water
  3. 3
    تجفيفAfter drying over sodium sulfate
  4. 4
    تركيزthe filtrate is concentrated under reduced pressure
  5. 5
    أخرىthe resulting oil is purified by column chromatography over silica gel

الإجراء التجريبي

91 g (0.04 mole) of 2,2-dimethyl-3-(2',2'-dichlorovinyl)-cyclopropanecarboxylic acid chloride are added dropwise, whilst stirring, to 4.6 g (0.05 mole) of γ-picoline, 100 ml of absolute ether and 8.5 g (0.38 mole) of 2-benzyl-(α-vinyl)-benzyl alcohol at 0°-5° C. After having been stirred for 12 hours at 25° C., the reaction mixture is filtered and the filtrate is successively washed with 2 N sodium bicarbonate solution, 2 N hydrochloric acid and water. After drying over sodium sulfate, the filtrate is concentrated under reduced pressure and the resulting oil is purified by column chromatography over silica gel, using toluene as the eluant.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04344961uspto-grants-1982_08