Sodium Hydroxide → 2-Ethyl-6-methoxybenzaldehyde

HRID 254468

反応式

HRID 254468 の反応式
[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

  1. temperatureto reflux for 1 hour
  2. extractionThe aqueous phase was extracted with ethyl acetate
  3. washthe combined extracts washed with brine
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. customevaporated
  7. 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

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