Nitric Acid → 3-Bromo-2-nitrothiophene
反応式
[N+:1]([O-:4])(O)=[O:2].C(OC(=O)C)(=O)C.[Br:12][C:13]1[CH:17]=[CH:16][S:15][CH:14]=1>C(O)(=O)C>[Br:12][C:13]1[CH:17]=[CH:16][S:15][C:14]=1[N+:1]([O-:4])=[O:2]参加物
5
実験手順
7.4 ml of fuming nitric acid was slowly added to 92.1 ml of acetic acid under ice-cooling, followed by stirring for 10 minutes, and a solution of 52.1 ml of acetic anhydride containing 25 g of 3-bromothiophene was slowly added in such a manner that the bulk temperature did not exceed 10° C., followed by stirring at 10 ° C. for 2 hours. Ice was added to the reaction solution, and the resulting crystals were collected by filtration, and washed with water and diethyl ether/n-hexane=1/5 successively, to give 17.4 g of the title compound.
後処理
- temperaturecooling
- customdid not exceed 10° C.
- stirringby stirring at 10 ° C. for 2 hours
- additionIce was added to the reaction solution
- filtrationthe resulting crystals were collected by filtration
- washwashed with water and diethyl ether/n-hexane=1/5 successively
出典と根拠
- ORDレコード
- ord-4f032b09762d403b9ad74e2a78a53d80
- 出典データセット
- uspto-grants-2003_06
- 特許番号
- US06583138B1
反応ノート
読み込み中…