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Hydrochloric Acid → 2-(3-Methoxy-phenoxy)-3-oxo-succinic acid diethyl ester

HRID 1804785
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HRID 1804785 반응식
[O-]CC.[Na+].[CH2:5]([O:7][C:8](=[O:14])[C:9](OCC)=[O:10])[CH3:6].[CH2:15]([O:17][C:18](=[O:29])[CH2:19][O:20][C:21]1[CH:26]=[CH:25][CH:24]=[C:23]([O:27][CH3:28])[CH:22]=1)[CH3:16].Cl>C(OCC)C>[CH2:15]([O:17][C:18](=[O:29])[CH:19]([O:20][C:21]1[CH:26]=[CH:25][CH:24]=[C:23]([O:27][CH3:28])[CH:22]=1)[C:9](=[O:10])[C:8]([O:7][CH2:5][CH3:6])=[O:14])[CH3:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 7268Diethyl OxalateHCID 2723922Sodium ethoxideHCID 21506379Ethyl 2-(3-methoxyphenoxy)acetate

생성물 1

HCID 591526762-(3-Methoxy-phenoxy)-3-oxo-succinic acid diethyl ester

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

Sodium ethoxide (32.5 g, 454 mmol) is covered with 1 l of dry diethyl ether. Oxalic acid diethyl ester (55.2 ml, 416 mmol) is added drop wise within 20 min. After 30 min stirring at room temperature, the mixture is heated to reflux. A solution of (3-methoxy-phenoxy)-acetic acid ethyl ester (22) (79.5 g, 378 mmol) in 80 ml of dry diethyl ether is added drop wise within 30 min and the mixture is allowed to reflux for 1 hour. After cooling down to room temperature, the reaction mixture is poured on 2M HCl (400 ml)/ice (400 g) and extracted with diethyl ether. The organic layers are dried over sodium sulfate, filtrated and evaporated.

후처리

  1. temperaturethe mixture is heated to reflux
  2. temperatureto reflux for 1 hour
  3. temperatureAfter cooling down to room temperature
  4. extractionextracted with diethyl ether
  5. dry with materialThe organic layers are dried over sodium sulfate
  6. filtrationfiltrated
  7. customevaporated

출처 및 근거

ORD 기록
ord-30253a59fe34430986cd4358c6c094de
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08354431B2

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