Ethanol → Ethyl 4-chloro-3-hydroxybenzoate

HRID 560319

반응식

HRID 560319 반응식
[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]

참가 물질

7

반응물 5

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

생성물 1

HCID 58847555Ethyl 4-chloro-3-hydroxybenzoate

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4a040cbe21bc4ea195dca19635252c09
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08063099B2

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