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Hydrochloric Acid → 3-(Methoxycarbonyl)-4-methylbenzoic acid

HRID 2071149
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반응식

HRID 2071149 반응식
[CH:1]([C:3]1[CH:4]=[CH:5][C:6]([CH3:13])=[C:7]([CH:12]=1)[C:8]([O:10][CH3:11])=[O:9])=[O:2].[OH:14]OS([O-])=O.[K+].O.Cl>CN(C=O)C.CCOC(C)=O>[CH3:11][O:10][C:8]([C:7]1[CH:12]=[C:3]([CH:4]=[CH:5][C:6]=1[CH3:13])[C:1]([OH:14])=[O:2])=[O:9]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 19700886Methyl 5-formyl-2-methylbenzoateHCID 23707502Potassium hydroxy sulfite

생성물 1

HCID 220698023-(Methoxycarbonyl)-4-methylbenzoic acid

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 268 mg of the methyl 5-formyl-2-methylbenzoate and 1.08 g (1.76 mmol) of Oxone in 6 mL of DMF was stirred at r.t. for 16.75 h. Water, 1N HCl, and EtOAc were added, and the aqueous layer was extracted with EtOAc. The combined extracts were dried over Na2SO4, filtered, and concentrated, and 3-(methoxycarbonyl)-4-methylbenzoic acid, which was used for the next reaction without further purification.

후처리

  1. extractionthe aqueous layer was extracted with EtOAc
  2. dry with materialThe combined extracts were dried over Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated
  5. custom3-(methoxycarbonyl)-4-methylbenzoic acid, which was used for the next reaction without further purification

출처 및 근거

ORD 기록
ord-430dedf4208244fc83ed6b0850c8dd3a
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08299267B2

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