반응 #94083

ord-b41c8aabc0ed4695882d0191604779f4

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도under reflux
  2. 2
    온도The whole is then heated for another two hours
  3. 3
    온도under reflux
  4. 4
    기타The mixture obtained
  5. 5
    여과filtered
  6. 6
    workup.DISTILLATIONExcess diethyl ketone and the water present are distilled off

실험 절차

A mixture of 70 g of methyl vinyl ketone, 10 g of water and 0.1 g of hydroquinone is dripped in the course of one hour into a mixture of 400 g of diethyl ketone and 10 g of a 30% by weight methanolic solution of sodium methylate which is boiling under reflux. The whole is then heated for another two hours under reflux. The mixture obtained is neutralized with glacial acetic and then filtered. Excess diethyl ketone and the water present are distilled off and the residue is fractionated in vacuo. 81 g of 2,3,6-trimethyl-2-cyclohexen-1-one having a boiling point of 89° C. at 12 mm Hg and 9 g of 4-methyl-3-ethyl-2-cyclohexen-1-one having a boiling point of 102° C. at 12 mm Hg are obtained. The total yield of cyclohexenone is 65% with reference to methyl vinyl ketone.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04128728uspto-grants-1978_12