반응 #2314284

ord-9beabb29ff9a402cb93a67449f2ebe89

반응 조건

온도
125°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도150° C., all for 30 minutes each, then cooled to room temperature
  2. 2
    추출The reaction mixture is extracted between ethyl ether and water
  3. 3
    세척the combined organic layers are washed with brine
  4. 4
    건조dried over magnesium sulfate
  5. 5
    농축The solution is concentrated in vacuo
  6. 6
    여과the product is purified by silica gel filtration

실험 절차

To a solution of ketone 2E (R=4-Methyl-3-pentenyl) (10 g) in diethylene glycol (30 mL) is added potassium hydroxide (4.3 g) and hydrazine hydrate (4.5 mL). The solution is sequentially heated to 100° C., 125° C., and 150° C., all for 30 minutes each, then cooled to room temperature. The reaction mixture is extracted between ethyl ether and water, and the combined organic layers are washed with brine and dried over magnesium sulfate. The solution is concentrated in vacuo, and the product is purified by silica gel filtration using 20:1 hexanes:ethyl acetate as an eluent.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06413448B1uspto-grants-2002_07