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Sodium Iodide → HCID 178517845, 화합물

HRID 2106804
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HRID 2106804 반응식
[I-].[Na+].Cl[Si](C)(C)C.[F:8][C:9]1[C:10]([O:22]C)=[N:11][CH:12]=[C:13]([O:15][C:16]([F:21])([F:20])[CH:17]([F:19])[F:18])[CH:14]=1>C(#N)C.C(Cl)Cl>[F:8][C:9]1[C:10]([OH:22])=[N:11][CH:12]=[C:13]([O:15][C:16]([F:20])([F:21])[CH:17]([F:18])[F:19])[CH:14]=1
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참가 물질

6

반응물 3

HCID 5238Sodium IodideHCID 6397ChlorotrimethylsilaneHCID 14837013HCID 14837013, 화합물

생성물 1

HCID 178517845HCID 178517845, 화합물

시약·촉매·용매 2

HCID 6342Acetonitrile용매HCID 6344Dichloromethane용매

실험 절차

Sodium iodide (1.80 g, 12.0 mmol) and then chlorotrimethylsilane (1.5 ml, 11.8 mmol) were added to a solution of 3-fluoro-2-methoxy-5-(1,1,2,2-tetrafluoroethoxy)pyridine (1.65 g, 6.79 mmol) in 8 ml of acetonitrile with stirring and under nitrogen and the mixture was heated at reflux for 2 5 hours. It was then allowed to cool and was diluted with 20 ml of methylene chloride. The resulting solution was extracted with water and with saturated aqueous sodium hydroxide, dried over sodium sulfate, and concentrated by evaporation under reduced pressure to obtain the title compound as a solid. This was recrystallized from toluene to obtain 0.95 g of the product as a white solid. The proton nmr spectrum was consistent with the assigned structure.

후처리

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 2 5 hours
  3. temperatureto cool
  4. extractionThe resulting solution was extracted with water and with saturated aqueous sodium hydroxide
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated by evaporation under reduced pressure

출처 및 근거

ORD 기록
ord-81b3ec38246f49359ea141f79d32f6aa
출처 데이터셋
uspto-grants-1990_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04931452

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