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Ethylparaben → HCID 14549135、化合物

HRID 863360
ノート
印刷プレビュー

反応式

HRID 863360 の反応式
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]
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 3

HCID 8434EthylparabenHCID 24758Sodium hydrideHCID 11141895HCID 11141895、化合物

生成物 1

HCID 14549135HCID 14549135、化合物収率 95.5%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

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%.

後処理

  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)

出典と根拠

ORDレコード
ord-99579ead58cd4807acfde06c20561c8a
出典データセット
uspto-grants-1998_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05720898

反応ノート

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