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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
ノート
印刷プレビュー

反応式

HRID 2219163 の反応式
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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

反応条件

温度
110 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-58924aa2f7b047c5ba363410c9d71da0
出典データセット
uspto-grants-2008_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07414054B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート