Ethanol → Ethyl 4-iodobenzoate

HRID 1222

반응식

HRID 1222 반응식
[I:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][CH:3]=1.S(Cl)(Cl)=O.[CH2:15](O)[CH3:16]>>[CH2:15]([O:7][C:6](=[O:8])[C:5]1[CH:9]=[CH:10][C:2]([I:1])=[CH:3][CH:4]=1)[CH3:16]

참가 물질

4

반응물 3

HCID 702EthanolHCID 120854-Iodobenzoic acidHCID 24386Thionyl Chloride

생성물 1

HCID 142891Ethyl 4-iodobenzoate

실험 절차

To a suspension of 10 g (40.32 mmol) of 4-iodobenzoic acid in 100 ml absolute ethanol was added 2 ml thionyl chloride and the mixture was then heated at reflux for 3 hours. Solvent was removed in vacuo and the residue was dissolved in 100 ml ether. The ether solution was washed with saturated NaHCO3 and saturated NaCl solutions and dried (MgSO4). Solvent was then removed in vacuo and the residue kugelrohr distilled (100 degrees C.; 0.55 mm) to give the title compound as a colorless oil, PMR (CDCl3): δ1.42 (3H, t, J~7 Hz), 4.4 (2H, q, J~7 Hz), 7.8 (4H).

후처리

  1. temperaturethe mixture was then heated
  2. temperatureat reflux for 3 hours
  3. customSolvent was removed in vacuo
  4. dissolutionthe residue was dissolved in 100 ml ether
  5. washThe ether solution was washed with saturated NaHCO3 and saturated NaCl solutions
  6. dry with materialdried (MgSO4)
  7. customSolvent was then removed in vacuo
  8. distillationthe residue kugelrohr distilled (100 degrees C.; 0.55 mm)

출처 및 근거

ORD 기록
ord-6724f220dc7c4e89ac64b79ac6a33d74
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05723620

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