Ethanol → HCID 117599790、化合物

HRID 513234ノート

反応式

HRID 513234 の反応式
[Br:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[C:4]([I:11])[C:3]=1[O:12][CH3:13].OS(O)(=O)=O.[CH3:19][CH2:20]O>>[CH2:19]([O:7][C:6](=[O:8])[C:5]1[CH:9]=[CH:10][C:2]([Br:1])=[C:3]([O:12][CH3:13])[C:4]=1[I:11])[CH3:20]

参加物

4

反応物 3

HCID 702EthanolHCID 1118Sulfuric AcidHCID 117599765HCID 117599765、化合物

生成物 1

HCID 117599790HCID 117599790、化合物

実験手順

A mixture of 4-Bromo-2-iodo-3-methoxy-benzoic acid (12.0 g, 0.0336 mol) and conc.H2SO4 (20 mL) in EtOH (200 mL) is refluxed overnight. After reaction, evaporated out EtOH and the mixture is extracted with ethyl acetate (3×1000 mL). The combined organic phase is washed with water and brine, dried over Na2SO4, concentrated in vacuo, purified by column chromatography on silica gel eluted with petroleum ether/ethyl acetate=20:1 to afford the desired product as a colourless oil.

後処理

  1. customAfter reaction
  2. customevaporated out EtOH
  3. extractionthe mixture is extracted with ethyl acetate (3×1000 mL)
  4. washThe combined organic phase is washed with water and brine
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated in vacuo
  7. custompurified by column chromatography on silica gel
  8. washeluted with petroleum ether/ethyl acetate=20:1

出典と根拠

ORDレコード
ord-fa4fe8b8d67d4189ba8aaef0dc1b75be
出典データセット
uspto-grants-2015_08
特許番号
US09102684B2

反応ノート

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