Isoamyl Nitrite → Ethyl [(4-chloro-2-{[2-chloro-4-(ethylsulfonyl)phenyl]thio}phenyl)thio]acetate

HRID 910836ノート

反応式

HRID 910836 の反応式
[SH:1][CH2:2][C:3]([O:5][CH2:6][CH3:7])=[O:4].C(ON=O)CC(C)C.[Cl:16][C:17]1[CH:23]=[CH:22][C:20](N)=[C:19]([S:24][C:25]2[CH:30]=[CH:29][C:28]([S:31]([CH2:34][CH3:35])(=[O:33])=[O:32])=[CH:27][C:26]=2[Cl:36])[CH:18]=1>C(#N)C.O>[Cl:16][C:17]1[CH:23]=[CH:22][C:20]([S:1][CH2:2][C:3]([O:5][CH2:6][CH3:7])=[O:4])=[C:19]([S:24][C:25]2[CH:30]=[CH:29][C:28]([S:31]([CH2:34][CH3:35])(=[O:32])=[O:33])=[CH:27][C:26]=2[Cl:36])[CH:18]=1

参加物

6

反応物 3

HCID 8053Isoamyl NitriteHCID 12185Ethyl ThioglycolateHCID 673913764-Chloro-2-{[2-chloro-4-(ethylsulfonyl)phenyl]thio}aniline

生成物 1

HCID 86620103Ethyl [(4-chloro-2-{[2-chloro-4-(ethylsulfonyl)phenyl]thio}phenyl)thio]acetate

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6342Acetonitrile溶媒

反応条件

温度
60 °C

実験手順

Ethyl mercaptoacetate (0.11 ml) followed by isoamylnitrite (0.16 ml) were added to a solution of the product from step (iii) (0.35 g) in dry acetonitrile (20 ml) and heated at 60° C. for 10 h. The mixture was diluted with water, extracted with diethylether, the organics dried and evaporated under reduced pressure. The residue was purified by chromatography on silica eluting with isohexane/diethylether 1:1, yield 0.10 g.

後処理

  1. extractionextracted with diethylether
  2. customthe organics dried
  3. customevaporated under reduced pressure
  4. customThe residue was purified by chromatography on silica eluting with isohexane/diethylether 1:1, yield 0.10 g

出典と根拠

ORDレコード
ord-ec67782cf61649b6a1a16fef9e985863
出典データセット
uspto-grants-2011_09
特許番号
US08022248B2

反応ノート

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