Dimethylformamide → HCID 59244769、化合物
反応式
[CH3:1]N(C=O)C.[Br:6][C:7]1[CH:8]=[C:9]([NH:13][C:14](=[O:16])[CH3:15])[CH:10]=[CH:11][CH:12]=1.[H-].[Na+].CI>O>[Br:6][C:7]1[CH:8]=[C:9]([N:13]([CH3:1])[C:14](=[O:16])[CH3:15])[CH:10]=[CH:11][CH:12]=1参加物
6
実験手順
To a DMF solution (15 ml) of N-(3-bromo-phenyl)-acetamide (1.19 g) obtained in Step A, 60% oily sodium hydride (279 mg) was added, followed by stirring at room temperature for 10 minutes. To this, methyl iodide (434 μl) was added, followed by stirring at room temperature for 21 hours. To this, water (30 ml) was added, followed by extraction with ethyl acetate (30 ml×2), and the organic layer was dried over sodium sulfate. The sodium sulfate was filtered off, followed by purification by silica gel column chromatography (dichloromethane/methanol=200/1), to obtain the desired compound (1.20 g, 94%).
後処理
- stirringby stirring at room temperature for 21 hours
- extractionfollowed by extraction with ethyl acetate (30 ml×2)
- dry with materialthe organic layer was dried over sodium sulfate
- filtrationThe sodium sulfate was filtered off
- customfollowed by purification by silica gel column chromatography (dichloromethane/methanol=200/1)
出典と根拠
- ORDレコード
- ord-dda48dbea7d743c6b1506fd0214f322c
- 出典データセット
- uspto-grants-2011_09
- 特許番号
- US08022205B2
反応ノート
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