Acetyl chloride → Methyl 3-fluoro-4-nitrobenzoate
反応式
[C:1](Cl)(=O)C.[F:5][C:6]1[CH:7]=[C:8]([CH:12]=[CH:13][C:14]=1[N+:15]([O-:17])=[O:16])[C:9]([OH:11])=[O:10]>CO>[F:5][C:6]1[CH:7]=[C:8]([CH:12]=[CH:13][C:14]=1[N+:15]([O-:17])=[O:16])[C:9]([O:11][CH3:1])=[O:10]参加物
4
実験手順
To a solution prepared by the dropwise addition of 12 ml acetyl chloride to 150 ml methanol was added 7.0 grams 3-fluoro-4-nitrobenzoic acid and the resulting mixture was stirred at room temperature for 18 hours. The solvent was removed in vacuo and the residue was partitioned between ethyl acetate and 2% sodium carbonate solution. The organic layer was washed with saturated sodium chloride solution, dried over magnesium sulfate, filtered, and evaporated in vacuo to give 6 grams of methyl 3-fluoro-4-nitrobenzoate as an orange oil which gradually hardened to a yellow solid.
後処理
- customThe solvent was removed in vacuo
- customthe residue was partitioned between ethyl acetate and 2% sodium carbonate solution
- washThe organic layer was washed with saturated sodium chloride solution
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- customevaporated in vacuo
出典と根拠
- ORDレコード
- ord-05ac5c8e382847e08303bf53883c12df
- 出典データセット
- uspto-grants-1997_04
- 特許番号
- US05624957
反応ノート
読み込み中…