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Ethylparaben → HCID 19890431、化合物

HRID 893542
ノート
印刷プレビュー

反応式

HRID 893542 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.[Na].[H-]>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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 8434EthylparabenHCID 166653HydrideHCID 5360545SodiumHCID 14533171HCID 14533171、化合物

生成物 1

HCID 19890431HCID 19890431、化合物収率 42%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒3 回

反応条件

温度
130 °C

実験手順

0.54 g of 3-trifluoromethylheptyl p-toluenesulfonate obtained in Step 1), 0.27 g of ethyl p-hydroxybenzoate and 1 ml of dimethylformamide (DMF) were placed in a round-bottomed flask, and 0.07 g of sodium 60%-hydride was added thereto together with DMF, followed by 6 hours of stirring at 130° C. After the reaction, DMF was distilled off under a reduced pressure, and water was added, followed by extraction with diethyl ether. The ether solution was dried with sodium sulfate, followed by distilling-off of the solvent to obtain 0.62 g of a crude product. The crude product was then purified by thin layer chromatography with benzene as the developer to obtain 0.22 g of ethyl p-(3-trifluoromethylheptyloxy)benzoate (yield: 42%).

後処理

  1. distillationwas distilled off under a reduced pressure, and water
  2. additionwas added
  3. extractionfollowed by extraction with diethyl ether
  4. dry with materialThe ether solution was dried with sodium sulfate
  5. customto obtain 0.62 g of a crude product
  6. customThe crude product was then purified by thin layer chromatography with benzene as the developer

出典と根拠

ORDレコード
ord-b24b2185bfd44cacbbe3152e807ab4ac
出典データセット
uspto-grants-1992_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05126071

反応ノート

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