Oxalyl chloride → (2-Bromo-5-methoxy-4-methyl-phenyl)-acetic acid chloride
反応式
[Br:1][C:2]1[CH:7]=[C:6]([CH3:8])[C:5]([O:9][CH3:10])=[CH:4][C:3]=1[CH2:11][C:12]([OH:14])=O.C(Cl)(=O)C([Cl:18])=O>ClCCl.CN(C=O)C>[Br:1][C:2]1[CH:7]=[C:6]([CH3:8])[C:5]([O:9][CH3:10])=[CH:4][C:3]=1[CH2:11][C:12]([Cl:18])=[O:14]参加物
5
実験手順
To a solution of (2-bromo-5-methoxy-4-methyl-phenyl)-acetic acid (149.4 mg) in dichloromethane (1.8 mL) was added oxalyl chloride (0.055 mL) followed by DMF (1 drop) uder argon. Mixture was stirred at rt for 3 h. Mixture was concentrated to dryness. Dichloroethane (ca. 10 mL) was added, and the mixture was back concentrated to dryness to obtain crude (2-bromo-5-methoxy-4-methyl-phenyl)-acetic acid chloride (151 mg).
後処理
- concentrationMixture was concentrated to dryness
- additionDichloroethane (ca. 10 mL) was added
- concentrationthe mixture was back concentrated to dryness
出典と根拠
- ORDレコード
- ord-ac473a77240f48d9a5d40899e3546efe
- 出典データセット
- uspto-grants-2012_04
- 特許番号
- US08153808B2
反応ノート
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