Methanol → Methyl 2-chloro-6-methylbenzoate
반응식
[Cl:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([CH3:11])[C:3]=1[C:4]([OH:6])=[O:5].[CH3:12]O>S(=O)(=O)(O)O>[Cl:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([CH3:11])[C:3]=1[C:4]([O:6][CH3:12])=[O:5]참가 물질
4
실험 절차
A mixture of 2-chloro-6-methylbenzoic acid (4.0 g, 23.4 mmol) in methanol (50 mL) and a few drops of concentrated sulfuric acid were stirred at reflux for 5 hours. After cooling to room temperature, methanol was evaporated, and the residue was dissolved in ethyl acetate (50 mL). The solution was extracted with saturated NaHCO3 (3×50 mL). The organic layer was dried over MgSO4, filtered, evaporated, and dried in vacuo, affording methyl 2-chloro-6-methylbenzoate (3.07 g, 71% yield). The product was used without further purification.
후처리
- temperatureat reflux for 5 hours
- custommethanol was evaporated
- dissolutionthe residue was dissolved in ethyl acetate (50 mL)
- extractionThe solution was extracted with saturated NaHCO3 (3×50 mL)
- dry with materialThe organic layer was dried over MgSO4
- filtrationfiltered
- customevaporated
- customdried in vacuo
출처 및 근거
- ORD 기록
- ord-77874ba847814ae18ab1c5d0517edcc4
- 출처 데이터셋
- uspto-grants-2015_05
- 특허 번호
- US09040538B2
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