Acetic Anhydride → N-(3-fluoro-2-formyl-phenyl)-acetamide
反応式
[NH2:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([F:10])[C:3]=1[CH:4]=[O:5].[C:11](OC(=O)C)(=[O:13])[CH3:12].C([O-])([O-])=O.[Na+].[Na+]>O>[F:10][C:6]1[C:3]([CH:4]=[O:5])=[C:2]([NH:1][C:11](=[O:13])[CH3:12])[CH:9]=[CH:8][CH:7]=1参加物
5
反応条件
- 温度
- 70 °C
実験手順
1.37 g (9.85 mmol) 2-amino-6-fluoro-benzaldehyde are combined with 20 ml acetic anhydride and heated to 70° C. for 4 h. Then the reaction mixture is stirred into 200 ml dist. water, adjusted to pH 7 with Na2CO3 and extracted three times with 50 ml of ethyl acetate. Then the organic phase is dried with MgSO4, the solvent is eliminated in vacuo. The crude product is purified by column chromatography. The carrier material used is silica gel and the eluant used is a mixture of cyclohexane:ethyl acetate (80:20).
後処理
- extractionextracted three times with 50 ml of ethyl acetate
- dry with materialThen the organic phase is dried with MgSO4
- customThe crude product is purified by column chromatography
- additiona mixture of cyclohexane:ethyl acetate (80:20)
出典と根拠
- ORDレコード
- ord-e14bf518de48403ea3cdb852d790be81
- 出典データセット
- uspto-grants-2007_07
- 特許番号
- US07241769B2
反応ノート
読み込み中…