Water → 2-Chloro-N-methoxy-N-methylbenzamide
反応式
[Cl:1][C:2]1[CH:10]=[CH:9][CH:8]=[CH:7][C:3]=1[C:4](Cl)=[O:5].Cl.[CH3:12][NH:13][O:14][CH3:15].N1C=CC=CC=1.O>ClCCl>[Cl:1][C:2]1[CH:10]=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([N:13]([O:14][CH3:15])[CH3:12])=[O:5]参加物
6
実験手順
To a solution of 2-chlorobenzoyl chloride (8 g, 46 mmol) in dichloromethane (200 mL) at 0° C. was added N,O-dimethylhydroxylamine hydrochloride (4.9 g, 50 mmol) followed by pyridine (11 mL, 137 mmol). The mixture was stirred at room temperature for 16 hours. Water was added to the reaction mixture and organic layer was washed with brine, dried over magnesium sulfate and concentrated. Purification by chromatography on silica gel gave 2-chloro-N-methoxy-N-methylbenzamide (21) (7.8 g, 39.2 mmol, 85%) as clear oil.
後処理
- washwas washed with brine
- dry with materialdried over magnesium sulfate
- concentrationconcentrated
- customPurification by chromatography on silica gel
出典と根拠
- ORDレコード
- ord-b72fea5e90fd4ee0b7a6e5bfe9b98fa0
- 出典データセット
- uspto-grants-2014_05
- 特許番号
- US08735399B2
反応ノート
読み込み中…