반응 #92972

ord-f451d76dd022479d86c4d6ad57a6b1ae

반응 조건

온도
65°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The resulting reaction mixture
  2. 2
    추출extracted with 400 ml
  3. 3
    추출The ether extract
  4. 4
    세척was washed with 0.5N sodium hydroxide
  5. 5
    건조with water, dried over sodium sulfate
  6. 6
    workup.DISTILLATIONdistilled under reduced pressure
  7. 7
    workup.DISTILLATIONThe distillate which was collected at 120°-124° C./0.01 mm
  8. 8
    기타solidified at room temperature

실험 절차

To a mixture of 0.5 mole (75 g.) of m-trifluoromethylphenol, 1 mole (56 g.) of potassium hydroxide, 100 ml. of water and 400 ml. of isopropanol was added 0.6 mole (84 g.) of 1,4-dichloro-2-butanol with stirring at temperature below 55° C. The resulting reaction mixture was heated at 65° C. for 20 hr., mixed with 2 liters of water, and extracted with 400 ml. of isopropyl ether. The ether extract was washed with 0.5N sodium hydroxide and then with water, dried over sodium sulfate and distilled under reduced pressure. The distillate which was collected at 120°-124° C./0.01 mm. solidified at room temperature and melted at 50°-52° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04609735uspto-grants-1986_09