반응식
[Br:1][C:2]1[CH:3]=[C:4]([CH:11]=[CH:12][C:13]=1[O:14][CH:15]([CH3:17])[CH3:16])[C:5]([O:7]C(C)C)=[O:6]>C(O)C.[OH-].[Na+]>[Br:1][C:2]1[CH:3]=[C:4]([CH:11]=[CH:12][C:13]=1[O:14][CH:15]([CH3:17])[CH3:16])[C:5]([OH:7])=[O:6]참가 물질
4
실험 절차
A solution of 1-methylethyl 3-bromo-4-[(1-methylethyl)oxy]benzoate (D14) (2.36 g, 7.84 mmol) in ethanol (100 mL) and aqueous sodium hydroxide (2M, 39 mL) was heated to reflux for 5 h. The reaction mixture was concentrated in vacuo and partitioned between ethyl acetate (125 mL) and water (125 mL), the latter acidified with 2M HCl (40 mL). The aqueous layer was extracted with further ethyl acetate (70 mL) and the combined organic extracts dried (phase separator) and concentrated in vacuo to give the title compound as an off-white solid (1.83 g, 7.06 mmol). MS (ES): C10H11BrO3 requires 258, 260; found 257, 259 (M−H+).
후처리
- temperatureto reflux for 5 h
- concentrationThe reaction mixture was concentrated in vacuo
- custompartitioned between ethyl acetate (125 mL) and water (125 mL)
- extractionThe aqueous layer was extracted with further ethyl acetate (70 mL)
- customthe combined organic extracts dried (phase separator)
- concentrationconcentrated in vacuo
출처 및 근거
- ORD 기록
- ord-23edd38d5d7844e28be7704ea492dfc1
- 출처 데이터셋
- uspto-grants-2012_12
- 특허 번호
- US08324254B2
연결된 노트
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