Sodium Hydroxide → 5,5-dimethyl-2,3,4,5-tetrahydro-1H-1-benzazepine
反応式
[CH3:1][CH:2]([CH3:14])[CH:3](O)[CH2:4][CH2:5][NH:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.[OH-].[Na+]>OS(O)(=O)=O>[CH3:1][C:2]1([CH3:14])[CH2:3][CH2:4][CH2:5][NH:6][C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][C:8]1=2参加物
4
反応条件
- 温度
- 50 °C
実験手順
A mixture of 4-methyl-1-(phenylamino)-pentan-3-ol (22 g, 0.11 mol) in 98% H2SO4 (250 mL) was stirred at 50° C. for 30 min. The reaction mixture was poured into ice-water basified with sat. NaOH solution to pH 8 and extracted with CH2Cl2. The combined organic phases were washed with brine, dried over Na2SO4, filtered and concentrated. The residue was purified by column chromatography (petroleum ether) to afford 5,5-dimethyl-2,3,4,5-tetrahydro-1H-benzo[b]azepine as a brown oil (1.5 g, 8%).
後処理
- extractionextracted with CH2Cl2
- washThe combined organic phases were washed with brine
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
- customThe residue was purified by column chromatography (petroleum ether)
出典と根拠
- ORDレコード
- ord-fd59111e5e29450495782abee9b9b131
- 出典データセット
- uspto-grants-2012_01
- 特許番号
- US08101767B2
反応ノート
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