Methanol → Methyl 4-(hydroxymethyl)-3-nitrobenzoate
반응식
[OH:1][CH2:2][C:3]1[CH:11]=[CH:10][C:6]([C:7]([OH:9])=[O:8])=[CH:5][C:4]=1[N+:12]([O-:14])=[O:13].[CH3:15]O>OS(O)(=O)=O>[CH3:15][O:8][C:7](=[O:9])[C:6]1[CH:10]=[CH:11][C:3]([CH2:2][OH:1])=[C:4]([N+:12]([O-:14])=[O:13])[CH:5]=1참가 물질
4
반응 조건
- 온도
- 70 °C
실험 절차
4-Hydroxymethyl-3-nitro-benzoic acid (step (a), 2.0 g, 10.2 mmol) was dissolved in 100 mL of MeOH, treated with 10 drops of concentrated H2SO4 and stirred at 70° C. After 36 h, the solution was concentrated in vacuo and redissolved in EtOAc. The EtOAc solution was washed with 1N NaOH and brine, dried over MgSO4, and concentrated to afford the title compound as a light-yellow solid upon drying under vacuum. MS m/z: 210.1 (M−1).
후처리
- concentrationthe solution was concentrated in vacuo
- dissolutionredissolved in EtOAc
- washThe EtOAc solution was washed with 1N NaOH and brine
- dry with materialdried over MgSO4
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-91887a49dcbf4a5ebbb0ffbfe966507f
- 출처 데이터셋
- uspto-grants-2004_11
- 특허 번호
- US06822097B1
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