Methanol → Methyl 2-(2-iodophenyl)acetate

HRID 1473022

반응식

HRID 1473022 반응식
[I:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:8][C:9]([OH:11])=[O:10].S(=O)(=O)(O)O.[CH3:17]O>>[I:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:8][C:9]([O:11][CH3:17])=[O:10]

참가 물질

4

반응 조건

온도
80 °C

실험 절차

2-(2-Iodophenyl)acetic acid (5.00 g, 19.1 mmol) was placed into a reaction flask and dissolved in MeOH (150 mL). Sulfuric acid (250 μL) was added and reaction mixture was stirred and heated at 80° C. under nitrogen for 16 hours. The resulting mixture was cooled to room temperature and the volatiles removed by evaporation under reduced pressure. The residue was taken up in ethyl acetate (100 mL), washed with 10% NaHCO3 (100 mL), dried (MgSO4) and evaporated under reduced pressure to give the title compound (I9) (5.20 g, 99%) as a clear liquid; 1H NMR (400 MHz, CDCl3) δ 7.85 (dd, J=7.9, 1.0 Hz, 1H), 7.35-7.27 (m, 2H), 6.97 (ddd, J=7.9, 7.0, 2.1 Hz, 1H), 3.81 (s, 2H), 3.72 (s, 3H).

후처리

  1. customreaction mixture
  2. temperatureThe resulting mixture was cooled to room temperature
  3. customthe volatiles removed by evaporation under reduced pressure
  4. washwashed with 10% NaHCO3 (100 mL)
  5. dry with materialdried (MgSO4)
  6. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-098ca4e4614c49398b82b3ba83cb4817
출처 데이터셋
uspto-grants-2015_04
특허 번호
US09012461B2

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