Bromine → HCID 19006175、化合物
反応式
[Br:1]Br.[Br:3][C:4]1[CH:5]=[C:6]([C:10]2[S:11][CH:12]=[CH:13][CH:14]=2)[CH:7]=[CH:8][CH:9]=1>C(O)(=O)C>[Br:1][C:12]1[S:11][C:10]([C:6]2[CH:7]=[CH:8][CH:9]=[C:4]([Br:3])[CH:5]=2)=[CH:14][CH:13]=1参加物
4
実験手順
A solution of bromine (8 g; 50 mM) in 20 mL of glacial acetic acid was added dropwise to a vigorously stirred solution of 2-(3'-bromophenyl)thiophene (12 g; 50 mM) in 80 mL of glacial acetic acid. The resulting mixture was heated to reflux 5 hrs, cooled and poured onto ice. A solid separated which was filtered and washed with ice water, and purified on silica gel using hexane as solvent to give 68% of 2-bromo-5-[3'-bromophenyl]thiophene as an amorphous solid.
後処理
- temperatureThe resulting mixture was heated
- temperatureto reflux 5 hrs
- temperaturecooled
- additionpoured onto ice
- customA solid separated which
- filtrationwas filtered
- washwashed with ice water
- custompurified on silica gel
出典と根拠
- ORDレコード
- ord-899f63392ae9462c9e82c9ba1bc39e3a
- 出典データセット
- uspto-grants-1994_03
- 特許番号
- US05292879
反応ノート
読み込み中…