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Tempo → 1-[1-[2-(tert-Butyldiphenylsiloxy)ethyl]cyclohexyl]acetaldehyde

HRID 1820294
ノート
印刷プレビュー

反応式

HRID 1820294 の反応式
CC1(C)N([O])C(C)(C)CCC1.[O:12]([CH2:30][CH2:31][C:32]1(CCO)[CH2:37][CH2:36][CH2:35][CH2:34][CH2:33]1)[Si:13]([C:26]([CH3:29])([CH3:28])[CH3:27])([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.[C:41](O)(=[O:43])[CH3:42].C(O)(=O)C.IC1C=CC=CC=1>C(Cl)Cl>[O:12]([CH2:30][CH2:31][C:32]1([C:41](=[O:43])[CH3:42])[CH2:37][CH2:36][CH2:35][CH2:34][CH2:33]1)[Si:13]([C:26]([CH3:28])([CH3:27])[CH3:29])([C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1)[C:20]1[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=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 2724126TempoHCID 12217721Iodo benzene diacetateHCID 574278602-[1-(2-tert-Butyldiphenylsiloxyethyl)cyclohexyl]ethanol

生成物 1

HCID 231098901-[1-[2-(tert-Butyldiphenylsiloxy)ethyl]cyclohexyl]acetaldehyde収率 160.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

After adding 2,2,6,6-tetramethylpiperidine 1-oxyl free radical (31 mg, 0.20 mmol) to a solution of 2-[1-[2-(tert-butyldiphenylsiloxy)ethyl]cyclohexyl]ethanol (810 mg, 1.97 mmol) and iodobenzene diacetate (700 mg, 2.17 mmol) in methylene chloride (10 mL), the mixture was stirred at room temperature for 4 hours. The reaction mixture was washed with saturated aqueous sodium hydrogencarbonate and saturated brine in that order and dried (anhydrous sodium sulfate), and then the solvent was distilled off under reduced pressure to obtain the title compound as a brown oil (1.29 g). This was used without purification for the following step.

後処理

  1. washThe reaction mixture was washed with saturated aqueous sodium hydrogencarbonate and saturated brine in that order
  2. dry with materialdried (anhydrous sodium sulfate)
  3. distillationthe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-e72eb954a3f44f64b8ee325944ed2115
出典データセット
uspto-grants-2009_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07601843B2

反応ノート

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