Acetyl chloride → Methyl 2-cyano-5-fluorobenzoate
反応式
[C:1]([C:3]1[CH:11]=[CH:10][C:9]([F:12])=[CH:8][C:4]=1[C:5]([OH:7])=[O:6])#[N:2].[C:13](Cl)(=O)C>CO>[CH3:13][O:6][C:5](=[O:7])[C:4]1[CH:8]=[C:9]([F:12])[CH:10]=[CH:11][C:3]=1[C:1]#[N:2]参加物
4
実験手順
To a stirred suspension of 16.0 g (96.9 mmol) 2-Cyano-5-fluoro-benzoic acid (Apollo) and 161 ml methanol were added 30.4 g (387.6 mmol) acetyl chloride drop wisely at 0° C. The reaction mixture was stirred over night, filtered and concentrated. The residue was diluted with dichloromethane, washed with diluted sodium hydrogen carbonate solution, dried with sodium sulphate and concentrated. The residue was purified by column chromatography (hexane:ethylacetate). The desired product 21a was obtained in 86.0 yield (14.9 g; 83.3 mmol)
後処理
- customdrop wisely at 0° C
- filtrationfiltered
- concentrationconcentrated
- additionThe residue was diluted with dichloromethane
- washwashed with diluted sodium hydrogen carbonate solution
- dry with materialdried with sodium sulphate
- concentrationconcentrated
- customThe residue was purified by column chromatography (hexane:ethylacetate)
出典と根拠
- ORDレコード
- ord-b4544c5bafe542a08fbebba62f443e07
- 出典データセット
- uspto-grants-2013_10
- 特許番号
- US08557776B2
反応ノート
読み込み中…