Chloroform → (3-Bromophenyl)thiourea
反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH:6]=[CH:7][CH:8]=1)[NH2:5].[S-:9][C:10]#[N:11].[NH4+].S([O-])(O)=O.[Na+].C(Cl)(Cl)Cl>Cl>[Br:1][C:2]1[CH:3]=[C:4]([NH:5][C:10]([NH2:11])=[S:9])[CH:6]=[CH:7][CH:8]=1参加物
6
反応条件
- 温度
- 100 °C
実験手順
A solution of 3-bromoaniline (10.89 ml, TCI) in 20% aqueous hydrochloric acid (18.2 ml) was added with ammonium thiocyanate (8.02 g, WAKO) and sodium hydrogensulfite (701 mg, WAKO), and stirred at 100° C. for 22 hours. The reaction mixture was added with chloroform (20 ml) for extraction, and the organic layer was dried. Then, the solvent was evaporated under reduced pressure. The residue was purified by column chromatography (Quad, hexane:ethyl acetate=2:1) to obtain the title compound (Intermediate 74, 4.45 g).
後処理
- customthe organic layer was dried
- customThen, the solvent was evaporated under reduced pressure
- customThe residue was purified by column chromatography (Quad, hexane:ethyl acetate=2:1)
出典と根拠
- ORDレコード
- ord-f027d3d982724b83aeca94ae33f97f83
- 出典データセット
- uspto-grants-2008_12
- 特許番号
- US07470807B2
反応ノート
読み込み中…