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

HRID 910836노트

반응식

HRID 910836 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 6342Acetonitrile용매

반응 조건

온도
60 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ec67782cf61649b6a1a16fef9e985863
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08022248B2

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