反应 #80586

ord-d86c6284680f4dd89004ee407d378b0c

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONwas added
  2. 2
    温度After heating
  3. 3
    温度to reflux the reaction mixture for 48 hours
  4. 4
    温度the reaction mixture was cooled
  5. 5
    过滤filtered
  6. 6
    洗涤The residue was washed with more acetone
  7. 7
    浓缩the combined filtrates were concentrated in vacuo
  8. 8
    其他The crude pale brown liquid (11.5 g) was chromatographed (silica gel, hexane/ethyl acetate, 85/15)

实验过程

To a mixture of 4-chlorophenol (6.1 g, 47.4 mmol) and potassium carbonate (13.1 g, 94.7 mmol) in acetone (200 mL), 2,3-dichloropropene (6.6 mL, 71 mmol) was added. After heating to reflux the reaction mixture for 48 hours, the reaction mixture was cooled and filtered. The residue was washed with more acetone and the combined filtrates were concentrated in vacuo. The crude pale brown liquid (11.5 g) was chromatographed (silica gel, hexane/ethyl acetate, 85/15) to give 1-(4-chlorophenoxy)-2-chloro-2-propene (8.9 g, 98%) as a white liquid: Anal. Calc'd. for C9H8OCl2 : C, 53.23, H, 3.97. Found: C, 53.09, H, 3.95.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05616601uspto-grants-1997_04