반응식
[I:1][C:2]1[CH:10]=[C:9]([O:11][CH3:12])[CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].S(=O)(=O)(O)O.[CH3:18]O>>[CH3:18][O:5][C:4](=[O:6])[C:3]1[CH:7]=[CH:8][C:9]([O:11][CH3:12])=[CH:10][C:2]=1[I:1]참가 물질
4
실험 절차
411 G. of 2-iodo-4-methoxy-benzoic acid, 4 l. methanol and 400 ml. of concentrated sulfuric acid are heated at reflux for 4 hours. The solution is then evaporated under reduced pressure, treated with water, and extracted with ether. The organic phase is then washed with aqueous sodium thiosulfate solution and aqueous sodium bicarbonate solution and subsequently dried over sodium sulfate. The solution is filtered, evaporated under reduced pressure and distilled. There is obtained the 2-iodo-4-methoxy-benzoic acid methyl ester, having a boiling point of 95°-98°/0.04 mm.
후처리
- temperatureat reflux for 4 hours
- customThe solution is then evaporated under reduced pressure
- additiontreated with water
- extractionextracted with ether
- washThe organic phase is then washed with aqueous sodium thiosulfate solution and aqueous sodium bicarbonate solution
- dry with materialsubsequently dried over sodium sulfate
- filtrationThe solution is filtered
- customevaporated under reduced pressure
- distillationdistilled
출처 및 근거
- ORD 기록
- ord-78bc88da641e4f408bf2b38b0b3f4b30
- 출처 데이터셋
- uspto-grants-1977_08
- 특허 번호
- US04044010
연결된 노트
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