Acetic Acid → 4-bromo-3-(2H-1,2,3-triazol-2-yl)thiophene-2-amine
反応式
[Br:1][C:2]1[C:3]([N:10]2[N:14]=[CH:13][CH:12]=[N:11]2)=[C:4]([N+:7]([O-])=O)[S:5][CH:6]=1.C(O)(=O)C>[Fe].O>[Br:1][C:2]1[C:3]([N:10]2[N:14]=[CH:13][CH:12]=[N:11]2)=[C:4]([NH2:7])[S:5][CH:6]=1参加物
5
実験手順
A mixture of 2-(4-bromo-2-nitrothiophen-3-yl)-2H-1,2,3-triazole (0.59 g, 2.15 mmol), iron powder (0.75 g, 13.38 mmol), glacial acetic acid (8.4 mL) and H2O (1.2 mL) was heated in an oil bath set at 70° C. under condenser with N2 (g) inlet for 1 h. Purification by flash chromatography (silica, 40:60 ethyl acetate/hexane) gave 4-bromo-3-(2H-1,2,3-triazol-2-yl)thiophene-2-amine (0.35 g, 66%). Retention time (min)=1.540, method [4], MS (ESI) 246.9 (M+H).
後処理
- temperaturewas heated in an oil bath
- customPurification by flash chromatography (silica, 40:60 ethyl acetate/hexane)
出典と根拠
- ORDレコード
- ord-e7f08422abb849b7aac32cac679e5641
- 出典データセット
- uspto-grants-2013_05
- 特許番号
- US08450363B2
反応ノート
読み込み中…