Aluminium lithium hydride → 2-(3-Ethoxyphenyl)ethan-1-amine
반응식
[H-].[H-].[H-].[H-].[Li+].[Al+3].[CH2:7]([O:9][C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([CH2:16][CH2:17][N+:18]([O-])=O)[CH:11]=1)[CH3:8]>C1COCC1>[CH2:7]([O:9][C:10]1[CH:11]=[C:12]([CH2:16][CH2:17][NH2:18])[CH:13]=[CH:14][CH:15]=1)[CH3:8]참가 물질
4
실험 절차
To a solution of LiAlH4 (1M in THF, 13 mL) was added dropwise a solution of 1-ethoxy-3-(2-nitro-ethyl)-benzene (0.5 g, 2.6 mmol) in THF (8 mL). The mixture was refluxed for two hours before allowing to cool and adding dropwise to rochelles salt. The mixture was extracted with ethyl acetate, dried with sodium sulfate and evaporated to dryness. The resulting yellow oil was purified by chromatography on silica, eluting with 3 to 15% MeOH/NH3 in dichloromethane, yielding the subtitled compound as a yellow oil (0.23 g).
후처리
- temperatureThe mixture was refluxed for two hours
- temperatureto cool
- additionadding dropwise to rochelles salt
- extractionThe mixture was extracted with ethyl acetate
- dry with materialdried with sodium sulfate
- customevaporated to dryness
- customThe resulting yellow oil was purified by chromatography on silica
- washeluting with 3 to 15% MeOH/NH3 in dichloromethane
출처 및 근거
- ORD 기록
- ord-36b41ebb896b47749e4443362d11c61f
- 출처 데이터셋
- uspto-grants-2009_03
- 특허 번호
- US07504392B2
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