Triethylamine → HCID 57736565、化合物
反応式
[Br:1][C:2]1[CH:9]=[C:8]([CH3:10])[C:7]([N+:11]([O-])=O)=[CH:6][C:3]=1[C:4]#[N:5].[Sn](Cl)(Cl)(Cl)Cl.C(N(CC)CC)C>C(O)C>[NH2:11][C:7]1[C:8]([CH3:10])=[CH:9][C:2]([Br:1])=[C:3]([CH:6]=1)[C:4]#[N:5]参加物
5
実験手順
To a solution of 2-bromo-4-methyl-5-nitrobenzonitrile (500 mg, 2.07 mmol) in ethanol (20 mL) was added tin chloride (785 mg, 4.14 mmol). The mixture was refluxed for 5 h. After cooling to room temperature, triethylamine (1.01 g, 10 mmol) was added. The mixture was concentrated and purified by silica chromatography (30-50% ethyl acetate in hexanes gradient) to afford 5-Amino-2-bromo-4-methylbenzonitrile a as beige solid; ESMS m/z 211 (M+H+).
後処理
- temperatureThe mixture was refluxed for 5 h
- concentrationThe mixture was concentrated
- custompurified by silica chromatography (30-50% ethyl acetate in hexanes gradient)
出典と根拠
- ORDレコード
- ord-08a4db77db524e80bf66e24c45ad1438
- 出典データセット
- uspto-grants-2014_10
- 特許番号
- US08859574B2
反応ノート
読み込み中…