Ammonium Chloride → 7-Fluoro-1H-indole
反応式
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N+:8]([O-])=O.[CH:11]([Mg]Cl)=[CH2:12].[Cl-].[NH4+]>O1CCCC1>[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]2[C:3]=1[NH:8][CH:12]=[CH:11]2参加物
5
反応条件
- 温度
- -50 °C
実験手順
2 Fluoronitrobenzene (20.0 g, 0.142 mol) was dissolved in dry tetrahydrofuran (400 ml) and cooled to -50° C. Vinylmagnesium chloride (288 ml, 15% wt/vol) was added at -45° C. and stirred at this temperature for one hour. Poured onto saturated ammonium chloride (600 ml). Separated and aqueous extracted with diethyl ether (2×200 ml). Dried (MgSO4), filtered and concentrated in vacuo to yield a dark oil which was purified by column chromatography on silica using toluene as mobile phase. Fractions concentrated to yield a crystalline solid.
後処理
- customSeparated
- extractionaqueous extracted with diethyl ether (2×200 ml)
- dry with materialDried (MgSO4)
- filtrationfiltered
- concentrationconcentrated in vacuo
- customto yield a dark oil which
- customwas purified by column chromatography on silica
- concentrationFractions concentrated
- customto yield a crystalline solid
出典と根拠
- ORDレコード
- ord-cab904f2e9934dfcbe038bb6b012a84e
- 出典データセット
- uspto-grants-1999_07
- 特許番号
- US05929072
反応ノート
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