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Dimethylformamide → HCID 21470422、化合物

HRID 2294748
ノート
印刷プレビュー

反応式

HRID 2294748 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:25]=[C:26]([C:36]([O:38][CH2:39][CH3:40])=[O:37])[C:27]([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)=[CH:28][CH:29]=1.CN(C)C=O.[H-].[Na+]>O>[CH2:21]([O:23][C:24]1[CH:25]=[C:26]([C:36]([O:38][CH2:39][CH3:40])=[O:37])[C:27]([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)=[CH:28][CH:29]=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

6

反応物 4

HCID 6228Dimethylformamide2 回HCID 24758Sodium hydrideHCID 9881286HCID 9881286、化合物HCID 11141895HCID 11141895、化合物

生成物 1

HCID 21470422HCID 21470422、化合物収率 86%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

The above-prepared 6.20 g (19.1 mM) of 10-undecenyl p-toluenesulfonate, 4.62 g (19.1 mM) of ethyl p-hydroxybiphenylcarboxylate and 6 ml of dimethylformamide (DMF) were mixed and sufficiently stirred. To the mixture, 0.77 g (19.3 mM) of 60% -sodium hydride was added, followed by heat-refluxing for 7 hours. After the reaction, the reaction mixture was subjected to distilling-off of DMF and addition of water, followed by extraction with ether to obtain an extract. The extract was dried with anhydrous sodium sulfate, followed by distilling-off of ether and purification by column chromatography (eluent: methylene chloride) to obtain 6.46 g (16.4 mM) of ethyl p-(10-undecenyl)oxybiphenylcarboxylate (Yield: 86%).

後処理

  1. temperatureby heat-refluxing for 7 hours
  2. customAfter the reaction
  3. extractionfollowed by extraction with ether
  4. customto obtain an extract
  5. dry with materialThe extract was dried with anhydrous sodium sulfate
  6. distillationfollowed by distilling-off of ether and purification by column chromatography (eluent: methylene chloride)

出典と根拠

ORDレコード
ord-a722a0376f494d4bb7e8612bfb28baf0
出典データセット
uspto-grants-1997_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05690858

反応ノート

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