Methanol → Methyl 2-iodo-3-nitrobenzoate

HRID 1639832

反応式

HRID 1639832 の反応式
[I:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].S(=O)(=O)(O)O.[CH3:19]O>>[I:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([O:6][CH3:19])=[O:5]

参加物

4

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 2209662-Iodo-3-nitrobenzoic acid

生成物 1

HCID 264093Methyl 2-iodo-3-nitrobenzoate収率 95%

実験手順

A mixture of 2-iodo-3-nitrobenzoic acid (31.0 g, 106 mmol) and concentrated sulfuric acid (24.9 mL, 317 mmol) in methanol (600 mL) was heated under reflux for 12 hr. The solvent was evaporated under reduced pressure and the residue was extracted with methylene chloride. The extract was washed with saturated aqueous sodium hydrogen carbonate solution and water, and dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by recrystallization (chloroform/hexane) to give the title compound (31.0 g, yield 95%).

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 12 hr
  3. customThe solvent was evaporated under reduced pressure
  4. extractionthe residue was extracted with methylene chloride
  5. washThe extract was washed with saturated aqueous sodium hydrogen carbonate solution and water
  6. dry with materialdried over anhydrous sodium sulfate
  7. customthe solvent was evaporated under reduced pressure
  8. customThe residue was purified by recrystallization (chloroform/hexane)

出典と根拠

ORDレコード
ord-3bbcf3c1b3e24be1a290d59631cecc6a
出典データセット
uspto-grants-2012_02
特許番号
US08110585B2

関連ノート

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