反応式
[CH2:1]([C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([O:9][CH3:10])[C:4]=1/[CH:11]=N/C(C(C)C)C(C)C)[CH3:2].[OH-:20].[Na+]>C1COCC1.Cl>[CH2:1]([C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([O:9][CH3:10])[C:4]=1[CH:11]=[O:20])[CH3:2]参加物
5
実験手順
A solution of 1.0 g (E)-[1-(2-ethyl-6-methoxy-phenyl)-methylidene]-(1-isopropyl-2-methyl-propyl)-amine in 1 ml THF and 0.19 ml 4N HCl was heated to reflux for 1 hour then cooled to ambient temperature and poured onto a 1N aqueous NaOH solution. The aqueous phase was extracted with ethyl acetate, the combined extracts washed with brine, dried over Na2SO4, filtered and evaporated. The residue was purified by flash-chromatography on silica gel with a heptane/ethyl acetate gradient as eluent: 0.50 g 2-ethyl-6-methoxy-benzaldehyde as colourless oil: MS (EI): 261.2 (M+.), 218.2 ((M-((CH3)2CH))+., 100%).
後処理
- temperatureto reflux for 1 hour
- extractionThe aqueous phase was extracted with ethyl acetate
- washthe combined extracts washed with brine
- dry with materialdried over Na2SO4
- filtrationfiltered
- customevaporated
- customThe residue was purified by flash-chromatography on silica gel with a heptane/ethyl acetate gradient as eluent
出典と根拠
- ORDレコード
- ord-cc2e1f364d6f465b9ca5dfe30ccda2b8
- 出典データセット
- uspto-grants-2011_01
- 特許番号
- US07875645B2
関連ノート
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