o-Phenetidine → 4-Bromo-2-ethoxyaniline
反応式
[Br:1]Br.[CH2:3]([O:5][C:6]1[CH:12]=[CH:11][CH:10]=[CH:9][C:7]=1[NH2:8])[CH3:4].[OH-].[K+]>C(O)(=O)C>[Br:1][C:11]1[CH:10]=[CH:9][C:7]([NH2:8])=[C:6]([O:5][CH2:3][CH3:4])[CH:12]=1参加物
5
実験手順
Over approximately 1 hour, 3 ml (58.4 mmol) of bromine dissolved in 20 ml of acetic acid is added dropwise to 7.8 ml (60 mmol, 1.03 eq) of 2-ethoxyaniline diluted in 20 ml of acetic acid. When all the bromine has been added, the precipitate formed is filtered on a Buchner funnel and rinsed with acetic acid. The hydrobromide is taken up in H2O, 5 g (90 mmol, 1.5 eq) of KOH pellets is added and extracted with CH2Cl2. The organic phase is dried on MgSO4 and the solvent is evaporated. The residue is purified by column chromatography (eluent CH2Cl2/pentane 9:1) to produce 7.52 g of the expected product as a brown oil (yield: 58%).
後処理
- customthe precipitate formed
- filtrationis filtered on a Buchner funnel
- washrinsed with acetic acid
- extractionextracted with CH2Cl2
- customThe organic phase is dried on MgSO4
- customthe solvent is evaporated
- customThe residue is purified by column chromatography (eluent CH2Cl2/pentane 9:1)
出典と根拠
- ORDレコード
- ord-21257b79279149a58b34946a4ac5b056
- 出典データセット
- uspto-grants-2007_07
- 特許番号
- US07238693B2
反応ノート
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