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Water → Ethyl [(2,2-diethoxyethyl)sulfanyl]acetate

HRID 1061663
ノート
印刷プレビュー

反応式

HRID 1061663 の反応式
[O-]CC.[Na+].[C:5]([O:9][CH2:10][CH3:11])(=[O:8])[CH2:6][SH:7].[CH2:12]([O:14][CH:15]([O:18][CH2:19][CH3:20])[CH2:16]Br)[CH3:13].O>C(O)C>[CH2:12]([O:14][CH:15]([O:18][CH2:19][CH3:20])[CH2:16][S:7][CH2:6][C:5]([O:9][CH2:10][CH3:11])=[O:8])[CH3:13]
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 962WaterHCID 12185Ethyl ThioglycolateHCID 74852Ethane, 2-bromo-1,1-diethoxy-HCID 2723922Sodium ethoxide

生成物 1

HCID 22284188Ethyl [(2,2-diethoxyethyl)sulfanyl]acetate収率 58.5%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Sodium ethoxide (2.83 g) is added to a solution of ethyl thioglycolate (5.00 g) and bromoacetaldehyde diethylacetal (8.20 g) in ethanol (150 ml), and the mixture is refluxed for three hours. The reaction mixture is allowed to stand at room temperature, water is added to the mixture, and the whole is extracted with diethyl ether. The extract is washed with saturated brine and dried over anhydrous magnesium sulfate. The extract is concentrated under reduced pressure, and the resulting residue is purified by silica gel column chromatography to give the titled reference compound (5.75 g).

後処理

  1. temperaturethe mixture is refluxed for three hours
  2. customto stand at room temperature
  3. extractionthe whole is extracted with diethyl ether
  4. washThe extract is washed with saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationThe extract is concentrated under reduced pressure
  7. customthe resulting residue is purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-98ee6c5626aa435387c98c317bbb2e7e
出典データセット
uspto-grants-2005_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06960575B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート