Methyl iodide → N,5-Dimethyl-2-nitroaniline
反応式
[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([N+:9]([O-:11])=[O:10])=[C:6]([NH2:8])[CH:7]=1.[H-].[Na+].I[CH3:15]>CN(C=O)C>[CH3:15][NH:8][C:6]1[CH:7]=[C:2]([CH3:1])[CH:3]=[CH:4][C:5]=1[N+:9]([O-:11])=[O:10]参加物
5
実験手順
To a solution of 5-methyl-2-nitro-phenylamine (3.04 g, 20.0 mmol) in anhydrous DMF (20 mL) at 0° C. was portionwise added 95% NaH (528 mg, 22.0 mmol) and the resulting mixture stirred for 10 min. A solution of iodomethane (1.25 mL, 20.0 mmol) in anhydrous DMF (10 mL) was then added. The ice bath was removed and the resulting mixture was stirred at room temperature overnight. The resulting mixture was diluted with water, the solid was collected by filtration, washed with H2O and hexanes to yield methyl-(5-methyl-2-nitro-phenyl)-amine MS 167 (M+1)+.
後処理
- customat 0° C.
- customThe ice bath was removed
- stirringthe resulting mixture was stirred at room temperature overnight
- additionThe resulting mixture was diluted with water
- filtrationthe solid was collected by filtration
- washwashed with H2O and hexanes
出典と根拠
- ORDレコード
- ord-0ad58647a4ca444ebe49bf7da12314ee
- 出典データセット
- uspto-grants-2015_03
- 特許番号
- US08981113B2
反応ノート
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