反应 #92972

ord-f451d76dd022479d86c4d6ad57a6b1ae

反应条件

温度
65°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The resulting reaction mixture
  2. 2
    萃取extracted with 400 ml
  3. 3
    萃取The ether extract
  4. 4
    洗涤was washed with 0.5N sodium hydroxide
  5. 5
    干燥with 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
    其他solidified at room temperature

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04609735uspto-grants-1986_09