Ethanol → Ethyl 4-chloro-3-hydroxybenzoate

HRID 560319ノート

反応式

HRID 560319 の反応式
[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][C:3]=1[OH:11].S(=O)(=O)(O)O.O.C([O-])(O)=O.[Na+].[CH3:23][CH2:24]O>CCOCC>[CH2:23]([O:7][C:6](=[O:8])[C:5]1[CH:9]=[CH:10][C:2]([Cl:1])=[C:3]([OH:11])[CH:4]=1)[CH3:24]

参加物

7

反応物 5

HCID 702EthanolHCID 962WaterHCID 1118Sulfuric AcidHCID 1418724-Chloro-3-hydroxybenzoic acidHCID 516892Sodium Bicarbonate

生成物 1

HCID 58847555Ethyl 4-chloro-3-hydroxybenzoate

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

A solution of 4-chloro-3-hydroxy-benzoic acid (29.3 mmol) in EtOH (110 mL) is treated with conc. sulfuric acid (23.6 mL) and heated to reflux for 16 h. Water (600 mL), NaHCO3 (100 g) and ether (300 mL) are added successively, the layers are separated and the aq. layer is extracted twice with ether. The combined organic layers are washed twice with brine, dried over MgSO4 and concentrated in vacuo to give the desired product which is used without further purification.

後処理

  1. temperatureheated
  2. temperatureto reflux for 16 h
  3. customthe layers are separated
  4. extractionthe aq. layer is extracted twice with ether
  5. washThe combined organic layers are washed twice with brine
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-4a040cbe21bc4ea195dca19635252c09
出典データセット
uspto-grants-2011_11
特許番号
US08063099B2

反応ノート

読み込み中…