Dimethylformamide → 2-Chloro-5-nitrobenzamide
反応式
[Cl:1][C:2]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][C:3]=1[C:4](O)=[O:5].ClCCl.C(Cl)(=O)C(Cl)=O.C[N:24](C)C=O>>[Cl:1][C:2]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][C:3]=1[C:4]([NH2:24])=[O:5]参加物
5
反応条件
- 温度
- 25 °C
実験手順
A mixture of 2-chloro-5-nitrobenzoic acid (15.0 g, 74.0 mmol) and 200 mL of dichloromethane was reacted with oxalyl chloride (16.2 mL, 186.0 mmol) and a catalytic amount of dimethylformamide. The mixture was stirred at 25° C. for 3 hours. The solvent was removed in vacuo, and the residue was redissolved in 200 mL of dichloromethane. The solution was cooled to 0° C., and ammonia was bubbled through the cold solution for 5 minutes, whereupon the product precipitated to form solution. The product was collected by filtration to yield 6.8 g, mp 174°-175° C.
後処理
- customThe solvent was removed in vacuo
- dissolutionthe residue was redissolved in 200 mL of dichloromethane
- temperatureThe solution was cooled to 0° C.
- customammonia was bubbled through the cold solution for 5 minutes, whereupon the product
- customprecipitated
- customto form solution
- filtrationThe product was collected by filtration
- customto yield 6.8 g, mp 174°-175° C.
出典と根拠
- ORDレコード
- ord-669072172d11414b8d8b946fb369fa91
- 出典データセット
- uspto-grants-1998_03
- 特許番号
- US05733921
反応ノート
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