반응 #215043

ord-75a878b802034342af05cac37840b8a4

반응 조건

온도
25°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONA mixture of 11.8 g
  2. 2
    세척of ether and washed with water, 5% sodium hydroxide solution and again with water to pH 8
  3. 3
    workup.DISTILLATIONThe mixture was then subjected to steam distillation in the presence of sodium bicarbonate solution at 20 torr for 2 hours
  4. 4
    기타to remove unreacted mesityl oxide and pinanyl hydroperoxide
  5. 5
    건조dried over anhydrous magnesium sulfate
  6. 6
    기타the ether removed under reduced pressure
  7. 7
    기타leaving 18.14 g

실험 절차

A mixture of 11.8 g. (0.12 mole) of mesityl oxide and 25.40 g. (0.15 mole) of pinanyl hydroperoxide was stirred at 0° C. while 2.0 g. of 77% sulfuric acid solution was slowly added. The reaction mixture was allowed to warm slowly to 25° C. and stirred for a total of 16 hours. The organic layer was taken up in 30 ml. of ether and washed with water, 5% sodium hydroxide solution and again with water to pH 8. The mixture was then subjected to steam distillation in the presence of sodium bicarbonate solution at 20 torr for 2 hours to remove unreacted mesityl oxide and pinanyl hydroperoxide. The product was taken up in ether, dried over anhydrous magnesium sulfate and the ether removed under reduced pressure leaving 18.14 g. of product (56.9% yield).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04257985uspto-grants-1981_03