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Water → HCID 53873583, 화합물

HRID 263470
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HRID 263470 반응식
[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]
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참가 물질

6

반응물 3

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

생성물 1

HCID 53873583HCID 53873583, 화합물

시약·촉매·용매 2

HCID 1118Sulfuric Acid촉매HCID 7918Acetic Anhydride용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-98b3f75389d14d12a14eb31b8910e4ca
출처 데이터셋
uspto-grants-1997_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05643925

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