Hydrogen Peroxide → 3-Methyl-1-oxo-5,6,7,8-tetrahydro-1lambda~5~-quinoline
반응식
[CH3:1][C:2]1[CH:3]=[N:4][C:5]2[CH2:6][CH2:7][CH2:8][CH2:9][C:10]=2[CH:11]=1.[OH:12]O>C(O)(=O)C>[CH3:1][C:2]1[CH:3]=[N+:4]([O-:12])[C:5]2[CH2:6][CH2:7][CH2:8][CH2:9][C:10]=2[CH:11]=1참가 물질
4
반응 조건
- 온도
- 80 °C
실험 절차
3-Methyl-5,6,7,8-tetrahydroquinoline (50 g.) was dissolved in glacial acetic acid (180 ml.) and the solution treated with 30% hydrogen peroxide (70 ml.) and heated at 80° C for 20 hours. The solvent was removed in vacuo and the residual oil diluted with water (25 ml.) and re-evaporated. The resulting oil was dissolved in chloroform (100 ml.), washed with aqueous sodium carbonate (2 × 25 ml.), saturated brine (2 × 25 ml.), dried (MgSO4) and the solvent removed in vacuo to give 3-Methyl-5,6,7,8-tetrahydroquinoline-1-oxide (60 g.) as a pale yellow solid which was used without purification.
후처리
- customThe solvent was removed in vacuo
- additionthe residual oil diluted with water (25 ml.)
- customre-evaporated
- dissolutionThe resulting oil was dissolved in chloroform (100 ml.)
- washwashed with aqueous sodium carbonate (2 × 25 ml.), saturated brine (2 × 25 ml.)
- dry with materialdried (MgSO4)
- customthe solvent removed in vacuo
출처 및 근거
- ORD 기록
- ord-746b476fc2664a33841b15201b862c89
- 출처 데이터셋
- uspto-grants-1977_03
- 특허 번호
- US04011229
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