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Ethylparaben → HCID 19890431、化合物

HRID 1460935
ノート
印刷プレビュー

反応式

HRID 1460935 の反応式
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
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 14533171HCID 14533171、化合物

生成物 1

HCID 19890431HCID 19890431、化合物収率 87.5%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

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%)

後処理

  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)

出典と根拠

ORDレコード
ord-0d93dd20d3574c51ba2ff48c53d014da
出典データセット
uspto-grants-1991_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05073306

反応ノート

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