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>>[CH2:16]([O:7][C:6](=[O:8])[C:5]1[CH:9]=[CH:10][C:2]([Br:1])=[C:3]([CH3:11])[CH:4]=1)[CH3:17]参加物
4
実験手順
To 4-bromo-3-methylbenzoic acid (3 g, 14 mmol) in EtOH (200 mL) was added thionyl chloride (2 mL, 25 mmol), and the reaction was stirred for 10 minutes. Additional thionyl chloride (3 mL, 35 mmol) was added, and the reaction was stirred overnight at 50° C. After cooling to room temperature, the mixture was quenched with the slow addition of powdered Na2CO3, and then filtered and concentrated. The residue was partitioned between EtOAc and H2O, and the organic layer was dried, filtered, and concentrated to give the title compound.
後処理
- stirringthe reaction was stirred overnight at 50° C
- customthe mixture was quenched with the slow addition of powdered Na2CO3
- filtrationfiltered
- concentrationconcentrated
- customThe residue was partitioned between EtOAc and H2O
- customthe organic layer was dried
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-aef2c2dc02544837b83e32250d5b87e9
- 出典データセット
- uspto-grants-2011_11
- 特許番号
- US08067445B2
反応ノート
読み込み中…