Water → HCID 21098652, 화합물

HRID 1351293노트

반응식

HRID 1351293 반응식
[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

참가 물질

6

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 21098651HCID 21098651, 화합물

생성물 1

HCID 21098652HCID 21098652, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-4f10437ee19f4460a7fe0cc869648448
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07217723B2

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