반응 #1747866

ord-eee27b9e4fe147dd8e55086696d664d8

반응 방정식

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

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was heated
  2. 2
    온도to reflux temperature
  3. 3
    온도heated
  4. 4
    여과the reaction mixture was filtered
  5. 5
    농축The filtrate was concentrated
  6. 6
    온도cooled in an ice bath, in the course of which a solid
  7. 7
    기타precipitated out
  8. 8
    기타This was removed by means of a blue-band filter
  9. 9
    기타dried
  10. 10
    기타The crude product (23.22 g) was recrystallized from 70 ml of ethanol
  11. 11
    기타an m.p. of 61-62° C. (lit. 62° C.)
  12. 12
    기타were obtained

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08029919B2uspto-grants-2011_10