2-(2-Nitrophenyl)-3-(trimethylsilyl)-2-propene → 2-(1-Methyl-2-trimethylsilylethyl)phenylamine
反応式
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[C:10](=[CH:12][Si:13]([CH3:16])([CH3:15])[CH3:14])[CH3:11])([O-])=O.[H][H]>O1CCCC1.[Pd]>[NH2:1][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[CH:10]([CH2:12][Si:13]([CH3:15])([CH3:14])[CH3:16])[CH3:11]参加物
5
実験手順
The reaction product of step A [7.2 g] was hydrogenated in tetrahydrofurane over palladium on charcoal at atmospheric pressure and room temperature until the uptake of hydrogen ceased. The catalyst was filtered off and, after evaporation of the solvent, the product was chromatographed on silacagel (eluent: 10% ethylacetate in hexane) to yield 2-(2-aminophenyl)-3-(trimethylsilyl)-propane [4.7 g; 88% purity according to NMR]. This product was used in the next step without further purification.
後処理
- filtrationThe catalyst was filtered off
- customafter evaporation of the solvent
- customthe product was chromatographed on silacagel (eluent: 10% ethylacetate in hexane)
出典と根拠
- ORDレコード
- ord-62388dac03b24cc1990f6196e9532ce6
- 出典データセット
- uspto-grants-2010_08
- 特許番号
- US07767623B2
反応ノート
読み込み中…