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Methyl iodide → HCID 22106697, 화합물

HRID 1456342
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HRID 1456342 반응식
[S:1]1[CH:5]=[CH:4][N:3]=[C:2]1[C:6]([C:12]1[S:13][CH:14]=[CH:15][N:16]=1)([OH:11])[C:7]([F:10])([F:9])[F:8].[H-].[Na+].[CH3:19]I>C(COC)OC>[CH3:19][O:11][C:6]([C:12]1[S:13][CH:14]=[CH:15][N:16]=1)([C:2]1[S:1][CH:5]=[CH:4][N:3]=1)[C:7]([F:9])([F:10])[F:8]
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참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 9860114HCID 9860114, 화합물

생성물 1

HCID 22106697HCID 22106697, 화합물수율 90.2%

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매

실험 절차

1, 1-Di(2-thiazolyl) -2,2,2-trifluoroethanol (1 g) was added to a stirred suspension of sodium hydride (80%, 225 mg) in dry dimethoxyethane (50 ml) at 0° C. After 15 minutes, methyl iodide (2.1 g) was added dropwise. The mixture was allowed to warm to room temperature and was then left stirring overnight. The mixture was concentrated by evaporation, then poured into saturated aqueous sodium chloride solution and extracted with dichloromethane. The material thus obtained was purified by flash chromatography to give the title compound as a white solid (950 mg). M.p. 40°-41° C. 13C Nmr (CDCl3) 54.9, 82.9 (g, J 30 Hz), 122.2, 122.8 (q, J 287 Hz), 143.2 and 163.6 ppm. Found: C, 38.7; H, 2.4; N, 9.9. C9H7F3N2OS2 requires C, 38.6; H, 2.5; N, 10.0%

후처리

  1. waitwas then left
  2. concentrationThe mixture was concentrated by evaporation
  3. additionpoured into saturated aqueous sodium chloride solution
  4. extractionextracted with dichloromethane
  5. customThe material thus obtained
  6. customwas purified by flash chromatography

출처 및 근거

ORD 기록
ord-c8790352e6ee4f11b1b76e781d9976fd
출처 데이터셋
uspto-grants-1998_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05843971

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