반응식
O[C:2]1[C:10]([I:11])=[CH:9][C:8]([I:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].S([O:18][CH3:19])(OC)(=O)=O.[CH3:20]C(C)=O>>[I:11][C:10]1[C:2]([O:18][CH3:19])=[C:3]([CH:7]=[C:8]([I:12])[CH:9]=1)[C:4]([O:6][CH3:20])=[O:5]참가 물질
4
실험 절차
A mixture of 2-hydroxy-3,5-diiodobenzoic acid (3.9 g, 10.0 mmol) potassium carbonate (4.15 g, 30.0 mmol) and dimethyl sulfate (2.77 g, 22.0 mmol) in acetone (33 ml) was heated at reflux for 16 h, cooled and concentrated. The residue was dissolved in EtOAc and washed with water, brine, dried (Na2SO4), filtered and concentrated to give an off-white solid (4.2 g, quantitative yield).
후처리
- temperaturewas heated
- temperatureat reflux for 16 h
- temperaturecooled
- concentrationconcentrated
- dissolutionThe residue was dissolved in EtOAc
- washwashed with water, brine
- dry with materialdried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-e6ee1f4f5e034f97afe232c2fb260e3c
- 출처 데이터셋
- uspto-grants-2015_08
- 특허 번호
- US09095590B2
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