Acetic Acid → 3,5-Dibromopyridine-2-carboxylic acid
反応式
C([C:3]1[C:8]([Br:9])=[CH:7][C:6]([Br:10])=C[N:4]=1)#N.[C:11]([OH:14])(=[O:13])[CH3:12].S(=O)(=O)(O)O>O>[Br:10][C:6]1[C:12]([C:11]([OH:14])=[O:13])=[N:4][CH:3]=[C:8]([Br:9])[CH:7]=1参加物
5
反応条件
- 温度
- 140 °C
実験手順
2-Cyano-3,5-dibromopyridine (prepared in the above (2)) 3.27 g is added to a mixture of acetic acid 14 ml, sulfuric acid 14 ml and water 14 ml, and the mixture is refluxed at 140° C. for 4 hours. The reaction mixture is cooled and water is added thereto. The resulting precipitate is filtered and washed with water. The precipitate is dissolved in ether, washed and dried. The solvent is removed in vacuo and crystallized from a mixture of ether and hexane to give 3,5-dibromopyridine-2-carboxylic acid. mp 170–171° C.
後処理
- temperatureThe reaction mixture is cooled
- filtrationThe resulting precipitate is filtered
- washwashed with water
- dissolutionThe precipitate is dissolved in ether
- washwashed
- customdried
- customThe solvent is removed in vacuo
- customcrystallized from a mixture of ether and hexane
出典と根拠
- ORDレコード
- ord-c8f7d0c165bd4808a2e405c0309f4b35
- 出典データセット
- uspto-grants-2007_05
- 特許番号
- US07220736B2
反応ノート
読み込み中…