反応 #1747866

ord-eee27b9e4fe147dd8e55086696d664d8

反応方程式

Oc1ccc(I)cc1
4-iodophenol
ClCc1ccccc1
benzyl chloride
O=C([O-])[O-].[K+].[K+]
potassium carbonate
Ic1ccc(OCc2ccccc2)cc1
4-Iodophenyl benzyl ether

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度was heated
  2. 2
    温度to reflux temperature
  3. 3
    温度heated
  4. 4
    ろ過the reaction mixture was filtered
  5. 5
    濃縮The filtrate was concentrated
  6. 6
    温度cooled in an ice bath, in the course of which a solid
  7. 7
    その他precipitated out
  8. 8
    その他This was removed by means of a blue-band filter
  9. 9
    その他dried
  10. 10
    その他The crude product (23.22 g) was recrystallized from 70 ml of ethanol
  11. 11
    その他an m.p. of 61-62° C. (lit. 62° C.)
  12. 12
    その他were obtained

実験手順

A reaction mixture composed of 21.40 g (95.3 mmol) of 98% 4-iodophenol, 12.19 g (95.3 mmol) of 99% benzyl chloride, 20.73 g (150 mmol) of potassium carbonate and 250 ml of acetone was heated to reflux temperature and heated to boiling for 30 hours. After cooling to room temperature, the reaction mixture was filtered. The filtrate was concentrated and then cooled in an ice bath, in the course of which a solid precipitated out. This was removed by means of a blue-band filter and then dried. The crude product (23.22 g) was recrystallized from 70 ml of ethanol. 17.20 g (58% of theory) of colorless microcrystals having an m.p. of 61-62° C. (lit. 62° C.) were obtained.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08029919B2uspto-grants-2011_10