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

HRID 1295969ノート

反応式

HRID 1295969 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-9f16943a7f884981864baaab28f08279
出典データセット
uspto-grants-2007_07
特許番号
US07244730B2

反応ノート

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