Methylamine → 1-(benzo[b]thiophen-7-yl)-N-methylmethanamine
반응식
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=2참가 물질
5
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-8aaa18b0b5a44412abfae50677459ff9
- 출처 데이터셋
- uspto-grants-1988_04
- 특허 번호
- US04737516
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