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Sodium Thiosulfate → HCID 90047349, 화합물

HRID 1507560
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HRID 1507560 반응식
[F:1][C:2]1[C:3]([Si](C)(C)C)=[CH:4][CH:5]=[C:6]2[C:10]=1[N:9]([CH3:11])[C:8](=[O:12])[C:7]2([CH3:14])[CH3:13].[I:19]Cl.S([O-])([O-])(=O)=S.[Na+].[Na+]>ClCCl>[F:1][C:2]1[C:3]([I:19])=[CH:4][CH:5]=[C:6]2[C:10]=1[N:9]([CH3:11])[C:8](=[O:12])[C:7]2([CH3:14])[CH3:13]
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참가 물질

5

반응물 3

HCID 24477Sodium ThiosulfateHCID 24640Iodine chlorideHCID 90046406HCID 90046406, 화합물

생성물 1

HCID 90047349HCID 90047349, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 7-fluoro-1,3,3-trimethyl-6-(trimethylsilyl)indolin-2-one (9.9 g, 37.3 mmol) in dichloromethane (500 ml) at 0° C. was added iodine monochloride (37.3 ml, 37.3 mmol). The reaction mixture was warmed to room temperature and stirred for 16 hours. A saturated aqueous solution of sodium thiosulfate was added to the reaction mixture and the aqueous phase was extracted with dichloromethane. The combined organic layers were dried over sodium sulfate. The solvent was evaporated and the residue purified by silica gel chromatography using ethyl acetate/heptane as eluent. The title compound was obtained as off-white crystals (9.82 g).

후처리

  1. extractionthe aqueous phase was extracted with dichloromethane
  2. dry with materialThe combined organic layers were dried over sodium sulfate
  3. customThe solvent was evaporated
  4. customthe residue purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-885dffb7df454b93a87cef7ac9072069
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09221816B2

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