Water → N-[5-Bromo-3-(1-fluoro-1-methylethyl)-2-methoxyphenyl]-N,N-dimethylamine

HRID 1295969노트

반응식

HRID 1295969 반응식
C(N(S(F)(F)[F:7])CC)C.[Br:10][C:11]1[CH:12]=[C:13]([N:23]([CH3:25])[CH3:24])[C:14]([O:21][CH3:22])=[C:15]([C:17](O)([CH3:19])[CH3:18])[CH:16]=1.O>C(Cl)Cl>[Br:10][C:11]1[CH:16]=[C:15]([C:17]([F:7])([CH3:19])[CH3:18])[C:14]([O:21][CH3:22])=[C:13]([N:23]([CH3:25])[CH3:24])[CH:12]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 123472(Diethylamino)sulfur trifluorideHCID 589100492-[5-Bromo-3-(dimethylamino)-2-methoxyphenyl]-2-propanol

생성물 1

HCID 58910057N-[5-Bromo-3-(1-fluoro-1-methylethyl)-2-methoxyphenyl]-N,N-dimethylamine수율 67.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Diethylaminosulfur trifluoride (620 mg) was added to a solution of 2-[5-bromo-3-(dimethylamino)-2-methoxyphenyl]-2-propanol (1 g) in methylene chloride while stirring on ice. After stirring for an additional 30 minutes while cooling on ice, water was added, extraction was performed with ethyl acetate, and the organic layer was washed with brine and then dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure and the residue was purified by silica gel column chromatography (solvent: n-hexane-ethyl acetate) to yield the title compound (680 mg) as an oil.

후처리

  1. stirringAfter stirring for an additional 30 minutes
  2. additionwas added
  3. extractionextraction
  4. washthe organic layer was washed with brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationThe solvent was distilled off under reduced pressure
  7. customthe residue was purified by silica gel column chromatography (solvent: n-hexane-ethyl acetate)

출처 및 근거

ORD 기록
ord-9f16943a7f884981864baaab28f08279
출처 데이터셋
uspto-grants-2007_07
특허 번호
US07244730B2

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