Water → HCID 21098652、化合物

HRID 1351293ノート

反応式

HRID 1351293 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([OH:21])[CH2:9][N:10]([CH3:20])[S:11]([C:14]2[S:15][C:16]([Br:19])=[CH:17][CH:18]=2)(=[O:13])=[O:12])=[CH:4][CH:3]=1.[H-].[Na+].[CH3:24]I.O>CN(C)C=O>[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([O:21][CH3:24])[CH2:9][N:10]([CH3:20])[S:11]([C:14]2[S:15][C:16]([Br:19])=[CH:17][CH:18]=2)(=[O:12])=[O:13])=[CH:4][CH:3]=1

参加物

6

反応物 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 21098651HCID 21098651、化合物

生成物 1

HCID 21098652HCID 21098652、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 5-bromothiophene-2-sulfonic acid [2-(4-fluorophenyl)-2-hydroxyethyl]-methyl-amide (the compound of Preparation Example 71) (210 mg) in N,N-dimethylformamide (2 mL) was added 60% sodium hydride (32 mg). After stirring for 45 minutes, methyl iodide (100 μL) was added. Water was added, the solution was extracted with ethyl acetate. After washing the organic layer with saturated sodium chloride water, and then was dried with anhydrous sodium sulfate, the residue that was obtained upon removal of the solvent by evaporation was purified by silica gel column chromatography (hexane/ethyl acetate), and the title compound (110 mg) was obtained as a colorless oily matter.

後処理

  1. extractionthe solution was extracted with ethyl acetate
  2. washAfter washing the organic layer with saturated sodium chloride water
  3. dry with materialwas dried with anhydrous sodium sulfate
  4. customthe residue that was obtained upon removal of the solvent by evaporation
  5. customwas purified by silica gel column chromatography (hexane/ethyl acetate)

出典と根拠

ORDレコード
ord-4f10437ee19f4460a7fe0cc869648448
出典データセット
uspto-grants-2007_05
特許番号
US07217723B2

反応ノート

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