Methanol → Methyl 3-ethylbenzoate
반응식
OS(O)(=O)=O.[CH2:6]([C:8]1[CH:9]=[C:10]([CH:14]=[CH:15][CH:16]=1)[C:11]([OH:13])=[O:12])[CH3:7].[CH3:17]O>O>[CH2:6]([C:8]1[CH:9]=[C:10]([CH:14]=[CH:15][CH:16]=1)[C:11]([O:13][CH3:17])=[O:12])[CH3:7]참가 물질
5
실험 절차
Concentrated H2SO4 (1.0 mL) was added to a solution of 3-ethylbenzoic acid (500 mg, 3.33 mmol) in MeOH (10 mL). The mixture was heated at reflux for 18 h then cooled to room temperature. The mixture was diluted with water (50 mL) and extracted with Et2O (3×100 mL). The combined organic phase was dried (Na2SO4), filtered and concentrated in vacuo. Purification of the crude residue by chromatography on silica gel (hexanes→20% EtOAc/hexanes, gradient) afforded 500 mg (91%) of methyl 3-ethylbenzoate.
후처리
- temperatureThe mixture was heated
- temperatureat reflux for 18 h
- extractionextracted with Et2O (3×100 mL)
- dry with materialThe combined organic phase was dried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated in vacuo
- customPurification of the crude residue by chromatography on silica gel (hexanes→20% EtOAc/hexanes, gradient)
출처 및 근거
- ORD 기록
- ord-2d3725fd1f9a4187a86fa47cc24da609
- 출처 데이터셋
- uspto-grants-2013_11
- 특허 번호
- US08592413B2
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