Methylamine → 1-(benzo[b]thiophen-7-yl)-N-methylmethanamine
反応式
Br[CH2:2][C:3]1[C:8]2[S:9][CH:10]=[CH:11][C:7]=2[CH:6]=[CH:5][CH:4]=1.[CH3:12][NH2:13]>ClCCl.C(O)C>[S:9]1[CH:10]=[CH:11][C:7]2[CH:6]=[CH:5][CH:4]=[C:3]([CH2:2][NH:13][CH3:12])[C:8]1=2参加物
5
実験手順
7-Bromomethylbenzo[b]thiophene is dissolved in dichloromethane, added to 40 ml of a 33% solution of methylamine in ethanol and allowed to stand overnight. The resulting mixture is concentrated and the residue taken up in dichloromethane and extracted with 2N HCl. The aqueous phase is made strongly basic with NaOH and shaken with dichloromethane. The organic phase is dried with potassium carbonate, concentrated by evaporation and the residue vacuum distilled to produce the title product as an oil. B.p.=103°/1.3 mbar.
後処理
- concentrationThe resulting mixture is concentrated
- extractionextracted with 2N HCl
- dry with materialThe organic phase is dried with potassium carbonate
- concentrationconcentrated by evaporation
- distillationthe residue vacuum distilled
出典と根拠
- ORDレコード
- ord-8aaa18b0b5a44412abfae50677459ff9
- 出典データセット
- uspto-grants-1988_04
- 特許番号
- US04737516
反応ノート
読み込み中…