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Ethylparaben → HCID 14549135, 화합물

HRID 863360
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HRID 863360 반응식
C1(C)C=CC(S(O[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH:20]=[CH2:21])(=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>[CH2:21]([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)[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16][CH2:15][CH2:14][CH2:13][CH:12]=[CH2:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8434EthylparabenHCID 24758Sodium hydrideHCID 11141895HCID 11141895, 화합물

생성물 1

HCID 14549135HCID 14549135, 화합물수율 95.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

6 ml of dimethylformamide was added to 6.20 g (19.1 mM) of 10-undecenyl p-toluenesulfonate and 3.17 g (19.1 mM) of ethyl p-hydroxybenzoate, followed by sufficient stirring. Into the resultant solution was added 0.77 g (19.3 mM) of sodium hydride (60%), followed by heat-refluxing for 7 hours. After the reaction, dimethylformamide was distilled off, followed by addition of water and extraction with ether. To the ether extract liquid was added anhydrous sodium sulfate for drying, followed by distilling-off of the ether and separation-purification by column chromatography (developer solvent: methylene chloride) to obtain 5.80 g (18.2 mM) of ethyl p-(10-undecenyl)oxybenzoate. Yield: 91.2%.

후처리

  1. temperatureby heat-refluxing for 7 hours
  2. distillationwas distilled off
  3. additionfollowed by addition of water and extraction with ether
  4. extractionTo the ether extract liquid
  5. additionwas added anhydrous sodium sulfate
  6. customfor drying
  7. distillationfollowed by distilling-off of the ether and separation-purification by column chromatography (developer solvent: methylene chloride)

출처 및 근거

ORD 기록
ord-99579ead58cd4807acfde06c20561c8a
출처 데이터셋
uspto-grants-1998_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05720898

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