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Isoamyl Nitrite → [[4-Chloro-2-[2-chloro-4-(methylsulfonyl)phenoxy]phenyl]thio]-acetic acid, ethyl ester

HRID 910845
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인쇄 미리보기

반응식

HRID 910845 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:22]=[CH:21][C:20](N)=[C:19]([O:24][C:25]2[CH:30]=[CH:29][C:28]([S:31]([CH3:34])(=[O:33])=[O:32])=[CH:27][C:26]=2[Cl:35])[CH:18]=1>C(#N)C.O>[Cl:16][C:17]1[CH:22]=[CH:21][C:20]([S:1][CH2:2][C:3]([O:5][CH2:6][CH3:7])=[O:4])=[C:19]([O:24][C:25]2[CH:30]=[CH:29][C:28]([S:31]([CH3:34])(=[O:32])=[O:33])=[CH:27][C:26]=2[Cl:35])[CH:18]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 8053Isoamyl NitriteHCID 12185Ethyl ThioglycolateHCID 692247814-Chloro-2-[2-chloro-4-(methylsulfonyl)phenoxy]-benzenamine

생성물 1

HCID 86620104[[4-Chloro-2-[2-chloro-4-(methylsulfonyl)phenoxy]phenyl]thio]-acetic acid, ethyl ester

시약·촉매·용매 2

HCID 962Water용매
HCID 6342
Acetonitrile
용매

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 example 15 step (i) (0.5 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 dichloromethane, yield 0.60 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 dichloromethane, yield 0.60 g

출처 및 근거

ORD 기록
ord-128fd2c3e0804c67a2b19c2fe223d30c
출처 데이터셋
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08022248B2

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