Ethanol → Ethyl 3-iodo-4-methylbenzoate

HRID 13752

反応式

HRID 13752 の反応式
[I:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[CH3:11])[C:5]([OH:7])=[O:6].S(=O)(=O)(O)O.[CH2:17](O)[CH3:18]>>[I:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[CH3:11])[C:5]([O:7][CH2:17][CH3:18])=[O:6]

参加物

4

反応物 3

HCID 702EthanolHCID 1118Sulfuric AcidHCID 6216403-Iodo-4-methylbenzoic acid

生成物 1

HCID 23073518Ethyl 3-iodo-4-methylbenzoate

実験手順

40.61 g of 3-iodo-4-methylbenzoic acid was suspended in 406 ml of ethanol and 9.1 ml of concentrated sulfuric acid was added, and then the mixture was heated at reflux for 24 hours. After the solvent was distilled off under reduced pressure, the residue was mixed with iced water, made basic with an aqueous saturated sodium hydrogen carbonate solution, followed by extraction with ethyl acetate twice. The extracts were washed in turn with water and saturated saline and then dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain 44.44 g of a crude product as a brown oily product.

後処理

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 24 hours
  3. distillationAfter the solvent was distilled off under reduced pressure
  4. additionthe residue was mixed with iced water
  5. extractionfollowed by extraction with ethyl acetate twice
  6. washThe extracts were washed in turn with water and saturated saline
  7. dry with materialdried over anhydrous magnesium sulfate
  8. distillationThe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-e7d713160acb4b798d7d7c899f2643a7
出典データセット
uspto-grants-2010_06
特許番号
US07728131B2

関連ノート

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