Methylamine → N-Methyl-4-nitrobenzamide
反応式
[N+:1]([C:4]1[CH:12]=[CH:11][C:7]([C:8](Cl)=[O:9])=[CH:6][CH:5]=1)([O-:3])=[O:2].[CH3:13][NH2:14].CCOC(C)=O>C1COCC1>[CH3:13][NH:14][C:8](=[O:9])[C:7]1[CH:11]=[CH:12][C:4]([N+:1]([O-:3])=[O:2])=[CH:5][CH:6]=1参加物
5
実験手順
4-Nitrobenzoyl chloride (7.00 g, 38 mmol, 1 eq) was dissolved in 50 ml of THF and added to a 2.0 M solution of methylamine in THF (41.5 ml, 83 mmol, 2.2 eq.) at 0° C. Worked up after 3 hours by adding EtOAc and rinsing 3× with 1N NaOH, 1× with brine. The organic layer was dried over MgSO4, then stripped to obtain 2.25 g of off-white solids as product. NMR (300 MHz, DMSO-d6) δ 8.80 (m, 1H), 8.33 (d, 2H, J=7 Hz), 8.06 (d, 2H, J=7 Hz). 2.86 (d, 3H, J=7 Hz).
後処理
- washrinsing 3× with 1N NaOH, 1× with brine
- dry with materialThe organic layer was dried over MgSO4
出典と根拠
- ORDレコード
- ord-374f943694a44131a1d1ea3d490082c3
- 出典データセット
- uspto-grants-2003_08
- 特許番号
- US06605623B1
反応ノート
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