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Water → HCID 53873583、化合物

HRID 977089
ノート
印刷プレビュー

反応式

HRID 977089 の反応式
[OH:1][C:2]1[CH:12]=[CH:11][C:5]([CH:6]=[CH:7][C:8]([OH:10])=[O:9])=[CH:4][C:3]=1[N+:13]([O-:15])=[O:14].O.[C:17](OCC)(=[O:19])[CH3:18]>C(OC(=O)C)(=O)C.S(=O)(=O)(O)O>[C:17]([O:1][C:2]1[CH:12]=[CH:11][C:5]([CH:6]=[CH:7][C:8]([OH:10])=[O:9])=[CH:4][C:3]=1[N+:13]([O-:15])=[O:14])(=[O:19])[CH3:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 962WaterHCID 8857Ethyl AcetateHCID 534017683-(4-Hydroxy-3-nitrophenyl)prop-2-enoic acid

生成物 1

HCID 53873583HCID 53873583、化合物

試薬・触媒・溶媒 2

HCID 1118Sulfuric Acid触媒HCID 7918Acetic Anhydride溶媒

実験手順

10 g of 4-hydroxy-3-nitrocinnamic acid (prepared as described in Preparation 1) were dissolved in 30 ml of acetic anhydride. One drop of sulfuric acid was added to the solution, which was then stirred for 2 hours at room temperature. 50 ml of water were added the solution, and it was then stirred for a further 2 hours. At the end of this time, ethyl acetate was added, and the mixture was washed with water and with a saturated aqueous solution of sodium chloride, in that order, and then dried over anhydrous sodium sulfate. The solvent was removed by distillation under reduced pressure, and the residue was mixed with toluene; the remaining acetic acid was removed by azeotropic distillation to obtain 10.2 g of the title compound as crystals.

後処理

  1. stirringwas then stirred for a further 2 hours
  2. washthe mixture was washed with water and with a saturated aqueous solution of sodium chloride, in that order
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solvent was removed by distillation under reduced pressure
  5. additionthe residue was mixed with toluene
  6. customthe remaining acetic acid was removed by azeotropic distillation

出典と根拠

ORDレコード
ord-b081a7d4bf8f4b9a95c74d12d050d0bf
出典データセット
uspto-grants-1997_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05614521

反応ノート

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