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2-(3'-Methoxy-3-nitro-biphenyl-4-yl)-malonic acid dimethyl ester → 3'-Methoxy-3-nitrobiphenyl-4-acetic acid

HRID 2219163
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반응식

HRID 2219163 반응식
C[O:2][C:3](=[O:26])[CH:4]([C:9]1[CH:14]=[CH:13][C:12]([C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([O:21][CH3:22])[CH:16]=2)=[CH:11][C:10]=1[N+:23]([O-:25])=[O:24])C(OC)=O>Cl>[CH3:22][O:21][C:17]1[CH:16]=[C:15]([C:12]2[CH:13]=[CH:14][C:9]([CH2:4][C:3]([OH:26])=[O:2])=[C:10]([N+:23]([O-:25])=[O:24])[CH:11]=2)[CH:20]=[CH:19][CH:18]=1
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참가 물질

3

반응물 1

HCID 106898032-(3'-Methoxy-3-nitro-biphenyl-4-yl)-malonic acid dimethyl ester

생성물 1

HCID 107556933'-Methoxy-3-nitrobiphenyl-4-acetic acid

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

반응 조건

온도
110 °C

실험 절차

2-(3′-Methoxy-3-nitro-biphenyl-4-yl)-malonic acid dimethyl ester (4.4023 gms.) is suspended in 45 mL of 6N HCl and heated at 110° C. for 4 days. The reaction mixture is cooled to room temperature and the precipitate is collected by filtration. As the solid material is in rather large chunks, the solid purification is simplified by first dissolving the solid chunks in an excess of hot methanol, and subsequently concentrating the solution in vacuo to get a more manageable powder. This powder is then triturated with approximately 10 mL of methanol and filtered yielding (3′-methoxy-3-nitro-biphenyl-4-yl)-acetic acid in the amount of 2.0120 gms.

후처리

  1. temperatureThe reaction mixture is cooled to room temperature
  2. filtrationthe precipitate is collected by filtration
  3. customthe solid purification
  4. dissolutionby first dissolving the solid chunks in an excess of hot methanol
  5. concentrationsubsequently concentrating the solution in vacuo
  6. customto get a more manageable powder
  7. customThis powder is then triturated with approximately 10 mL of methanol
  8. filtrationfiltered

출처 및 근거

ORD 기록
ord-58924aa2f7b047c5ba363410c9d71da0
출처 데이터셋
uspto-grants-2008_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07414054B2

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