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2,2-Bis-(2-phenylsulfanyl-ethyl)-malonic acid → 4-Phenylsulfanyl-2-(2-phenylsulfanyl-ethyl)-butyric acid

HRID 1830125
ノート
印刷プレビュー

反応式

HRID 1830125 の反応式
[C:1]1([S:7][CH2:8][CH2:9][C:10]([CH2:17][CH2:18][S:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)(C(O)=O)[C:11]([OH:13])=[O:12])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1>C(OCC)(=O)C>[C:20]1([S:19][CH2:18][CH2:17][CH:10]([CH2:9][CH2:8][S:7][C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[C:11]([OH:13])=[O:12])[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

3

反応物 1

HCID 220539352,2-Bis-(2-phenylsulfanyl-ethyl)-malonic acid

生成物 1

HCID 220540334-Phenylsulfanyl-2-(2-phenylsulfanyl-ethyl)-butyric acid収率 36.8%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

2,2-Bis-(2-phenylsulfanyl-ethyl)-malonic acid (5.628 g) was heated at 150° C. for 30 minutes. The reaction mixture was cooled to room temperature, dissolved in ethyl acetate and washed with aqueous sodium bicarbonate. The ethyl acetate solution was washed with saturated aqueous sodium chloride and then dried over magnesium sulfate. The solvent was removed by rotary evaporation at reduced pressure and the residue was chromatographed on silica gel eluting with ethyl acetate/hexane to give 4-phenylsulfanyl-2-(2-phenylsulfanyl-ethyl)-butyric acid (1.831 g).

後処理

  1. washwashed with aqueous sodium bicarbonate
  2. washThe ethyl acetate solution was washed with saturated aqueous sodium chloride
  3. dry with materialdried over magnesium sulfate
  4. customThe solvent was removed by rotary evaporation at reduced pressure
  5. customthe residue was chromatographed on silica gel eluting with ethyl acetate/hexane

出典と根拠

ORDレコード
ord-69426c290a3c4ecd8fd376473f6a19da
出典データセット
uspto-grants-2006_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07064123B1

反応ノート

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