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Ethylparaben → HCID 19890431, 화합물

HRID 1460935
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HRID 1460935 반응식
C1(C)C=CC(S(O[CH2:11][CH2:12][CH:13]([C:18]([F:21])([F:20])[F:19])[CH2:14][CH2:15][CH2:16][CH3:17])(=O)=O)=CC=1.[OH:23][C:24]1[CH:34]=[CH:33][C:27]([C:28]([O:30][CH2:31][CH3:32])=[O:29])=[CH:26][CH:25]=1.[H-].[Na+]>CN(C)C=O>[F:19][C:18]([F:20])([F:21])[CH:13]([CH2:14][CH2:15][CH2:16][CH3:17])[CH2:12][CH2:11][O:23][C:24]1[CH:25]=[CH:26][C:27]([C:28]([O:30][CH2:31][CH3:32])=[O:29])=[CH:33][CH:34]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8434EthylparabenHCID 24758Sodium hydrideHCID 14533171HCID 14533171, 화합물

생성물 1

HCID 19890431HCID 19890431, 화합물수율 87.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

In a round-bottomed flask, 0.88 g of the 3-trifluoromethylheptyl p-toluenesulfonate 2, 0.4 g of ethyl p-hydroxybenzoate and 1 ml of dimethylformamide were placed, and 50 mg of sodium hydride was added thereto, followed by 8 hours of heat-refluxing and 15 hours of standing at room temperature. After the reaction, dimethylformamide was distilled off, and dilute hydrochloric acid was added to the product, which was then extracted with methylene chloride. The resultant organic layer was washed with water and dried with magnesium sulfate, followed by distilling-off of the solvent and purification by thin layer chromatography (developer: methylene chloride/ hexane=1/1) to obtain 0.7 g of ethyl p-(3-trifluoromethylheptyloxy)benzoate 3. (Yield: 80%)

후처리

  1. temperatureof heat-refluxing and 15 hours
  2. customof standing at room temperature
  3. distillationwas distilled off
  4. additiondilute hydrochloric acid was added to the product, which
  5. extractionwas then extracted with methylene chloride
  6. washThe resultant organic layer was washed with water
  7. dry with materialdried with magnesium sulfate
  8. distillationfollowed by distilling-off of the solvent and purification by thin layer chromatography (developer: methylene chloride/ hexane=1/1)

출처 및 근거

ORD 기록
ord-0d93dd20d3574c51ba2ff48c53d014da
출처 데이터셋
uspto-grants-1991_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05073306

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