Water → HCID 97178977, 화합물

HRID 1526302

반응식

HRID 1526302 반응식
[Br:1][C:2]1[CH:6]=[CH:5][N:4]([CH2:7][CH2:8][OH:9])[N:3]=1.[H-].[Na+].I[CH3:13].O>CN(C)C=O>[Br:1][C:2]1[CH:6]=[CH:5][N:4]([CH2:7][CH2:8][O:9][CH3:13])[N:3]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 594022992-(3-bromo-1H-pyrazol-1-yl)ethan-1-ol

생성물 1

HCID 97178977HCID 97178977, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 2-(3-bromo-1H-pyrazol-1-yl)ethanol obtained in Step D of Example 6 (300 mg) in N,N-dimethylformamide (16 mL) were added sodium hydride (55%, 137 mg) and iodomethane (196 μL) under ice-cooling. The reaction mixture was stirred under ice-cooling for 2 hr, water was added thereto, and the mixture was extracted with ethyl acetate. The extract was dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (150 mg).

후처리

  1. temperaturecooling
  2. temperaturecooling for 2 hr
  3. extractionthe mixture was extracted with ethyl acetate
  4. dry with materialThe extract was dried over anhydrous sodium sulfate
  5. customthe solvent was evaporated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-71e9632191554930a2cd0d0635f241e0
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09085578B2

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