Hydrochloric Acid → 1-Nitro-2-phenylethane
反応式
[C:1]1([CH:7]=[CH:8][N+:9]([O-:11])=[O:10])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[BH4-].[Na+].Cl>C(Cl)(Cl)Cl.CC(O)C>[C:1]1([CH2:7][CH2:8][N+:9]([O-:11])=[O:10])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1参加物
5
実験手順
2-Phenylnitroethene (5.12 g, 34.3 mmol, from step 15a) was dissolved in CHCl3 /i-PrOH (410:85 mL) and SiO2 (51.4 g) was added. NaBH4 (5.2 g, 137 mmol) was added in portions, and the mixture was stirred for 90 minutes at room temperature. HCl (0.5N, 100, mL) was added, and the mixture was stirred for 30 minutes. The layers were separated, and the aqueous phase was extracted with methylene chloride. The organic layers were combine, dried (MgSO4) and concentrated. The residue was chromatographed on silica gel (eluting with ether:hexanes 1:30) to give the title compound as an oil (3.89 g, 75%).
後処理
- stirringthe mixture was stirred for 30 minutes
- customThe layers were separated
- extractionthe aqueous phase was extracted with methylene chloride
- dry with materialdried (MgSO4)
- concentrationconcentrated
- customThe residue was chromatographed on silica gel (eluting with ether:hexanes 1:30)
出典と根拠
- ORDレコード
- ord-d656571e780d4bccad9fd6471b2c4bc3
- 出典データセット
- uspto-grants-1998_03
- 特許番号
- US05733912
反応ノート
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