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Carbon Dioxide → HCID 68117788、化合物

HRID 597656
ノート
印刷プレビュー

反応式

HRID 597656 の反応式
[C:1]([O:4][C:5]1[CH:19]=[CH:18][C:8]([CH:9]=[C:10]([NH:14][C:15](=[O:17])[CH3:16])C(O)=O)=[CH:7][C:6]=1OC)(=[O:3])[CH3:2].[C:22](=O)=[O:23]>[Cu].N1C2C(=CC=CC=2)C=CC=1>[C:15]([NH:14][CH:10]=[CH:9][C:8]1[CH:7]=[CH:6][C:5]([O:4][C:1](=[O:3])[CH2:2][O:23][CH3:22])=[CH:19][CH:18]=1)(=[O:17])[CH3:16]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 280Carbon DioxideHCID 27543002-(Acetylamino)-3-[4-(acetyloxy)-3-methoxyphenyl]-2-propenoic acid

生成物 1

HCID 68117788HCID 68117788、化合物

試薬・触媒・溶媒 2

HCID 23978Copper触媒HCID 7047Quinoline溶媒

実験手順

18.0 g (0.06 mol) of 4-acetoxy-α-acetylamino-3-methoxy-cinnamic acid are heated with 30 ml of quinoline and 1.2 g of copper powder to 160°-170° C for 3 hours, in the course of which carbon dioxide is evolved. Thereafter, the quinoline is distilled off under reduced pressure and the residual mass is taken up in ethyl acetate. After filtering off the copper powder, the ethyl acetate solution is extracted with 25 ml of 1 N hydrochloric acid and is then washed with water and subsequently with sodium bicarbonate solution. The organic phase is dried over sodium sulphate and thereafter the solvent is removed by distillation under reduced pressure. The resulting oil yields 4-(2-acetylaminovinyl)-2-methoxy-acetoxy-benzene, of melting point 169°-170° C, from ethyl acetate.

後処理

  1. distillationThereafter, the quinoline is distilled off under reduced pressure
  2. filtrationAfter filtering off the copper powder
  3. extractionthe ethyl acetate solution is extracted with 25 ml of 1 N hydrochloric acid
  4. washis then washed with water and subsequently with sodium bicarbonate solution
  5. dry with materialThe organic phase is dried over sodium sulphate
  6. customthe solvent is removed by distillation under reduced pressure

出典と根拠

ORDレコード
ord-8a5624b696ed48938d95beb7a3d3c9c4
出典データセット
uspto-grants-1977_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04014920

反応ノート

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