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Ethanol → HCID 86617335、化合物

HRID 661748
ノート
印刷プレビュー

反応式

HRID 661748 の反応式
[Na].[C:2]1([SH:8])[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(O)C.[CH2:12]([O:19][N:20]=[C:21](Br)[CH:22]=[CH:23][S:24][C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>C(Cl)(Cl)Cl>[CH2:12]([O:19][N:20]=[C:21]([S:8][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[CH:22]=[CH:23][S:24][C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1
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 702EthanolHCID 7969ThiophenolHCID 5360545SodiumHCID 86617336N-benzyloxy-3-(phenylthio)acrylimidoyl bromide

生成物 1

HCID 86617335HCID 86617335、化合物収率 43%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

Sodium salt of thiophenol (0.14 g) was added to ethanol (5 ml) solution of N-benzyloxy-3-phenylthioacrylimidoyl bromide (0.30 g) at room temperature, then it was heat refluxing for three hours. It was cooled, and chloroform (50 ml) was added to the reaction mixture. It was successively washed with 1N aqueous sodium hydroxide solution, pure water, aqueous saturated sodium chloride solution. The organic layer was dried over anhydrous magnesium sulfate, concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=20:1) to obtain phenyl N-benzyloxy-3-(phenylthio)thioacrylimidate (0.14 g) as colorless oil.

後処理

  1. temperatureit was heat
  2. temperaturerefluxing for three hours
  3. temperatureIt was cooled
  4. washIt was successively washed with 1N aqueous sodium hydroxide solution, pure water, aqueous saturated sodium chloride solution
  5. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=20:1)

出典と根拠

ORDレコード
ord-a1f938d760964fd8b184aed082acbadb
出典データセット
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08084644B2

反応ノート

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