反応式
[N+:1]([C:4]1[CH:5]=[C:6]([CH2:10][CH2:11][OH:12])[CH:7]=[CH:8][CH:9]=1)([O-])=O.C([O-])=O.[NH4+]>CO.[Pd]>[NH2:1][C:4]1[CH:5]=[C:6]([CH2:10][CH2:11][OH:12])[CH:7]=[CH:8][CH:9]=1参加物
5
実験手順
2-(3-Nitrophenyl)ethanol (836 mg, 5.00 mmol) and Pd (10% on charcoal, 200 mg) were suspended in dry methanol (10 mL). After the addition of ammonium formate (1.450 g, 23 mmol) a slightly exothermic and effervescent reaction was observed. After stirring for 1 h at room temperature the mixture was filtered over celite. The filtrate was evaporated and the residue dissolved in ethyl acetate. After washing with saturated aqueous sodium hydrogencarboante solution, water and brine the organic layer was dried (magnesium sulfate) and the solvent removed under reduced pressure affording the title compound in 54% yield (373 mg) as a white solid.
後処理
- customeffervescent reaction
- filtrationwas filtered over celite
- customThe filtrate was evaporated
- dissolutionthe residue dissolved in ethyl acetate
- washAfter washing with saturated aqueous sodium hydrogencarboante solution, water and brine the organic layer
- dry with materialwas dried (magnesium sulfate)
- customthe solvent removed under reduced pressure
出典と根拠
- ORDレコード
- ord-824ab447f90a413daf02962ad5f273a6
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07732600B2
関連ノート
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