Ethanol → Ethyl 4-bromo-3-methylbenzoate
反応式
[Br:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][C:3]=1[CH3:11].S(Cl)(Cl)=O.[CH3:16][CH2:17]O>>[Br:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([O:8][CH2:16][CH3:17])=[O:7])=[CH:4][C:3]=1[CH3:11]参加物
4
実験手順
To a solution of 4-bromo-3-methylbenzoic acid (commercially available) (1.0 eq.) in EtOH (0.3 M) was added thionyl chloride (1.5 eq.) and heated to reflux for 2 hours. The solvent was concentrated en vacuo, and the residue was diluted in ether and neutralized with saturated aqueous sodium bicarbonate solution. The two phases were separated, and the aqueous layer was extracted with ether. The combined organic layers were washed with brine, dried over anhydrous MgSO4, and concentrated en vacuo to give ethyl 4-bromo-3-methylbenzoate.
後処理
- temperatureheated
- temperatureto reflux for 2 hours
- concentrationThe solvent was concentrated en vacuo
- additionthe residue was diluted in ether and neutralized with saturated aqueous sodium bicarbonate solution
- customThe two phases were separated
- extractionthe aqueous layer was extracted with ether
- washThe combined organic layers were washed with brine
- dry with materialdried over anhydrous MgSO4
- concentrationconcentrated en vacuo
出典と根拠
- ORDレコード
- ord-6ff0f0b8a91e4a0ba917b901c448c6e7
- 出典データセット
- uspto-grants-2014_11
- 特許番号
- US08895577B2
反応ノート
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