Ammonium Chloride → 5-(1-Hydroxy-2-methylpropyl)thiophene-3-sulfonic acid [2-(4-fluorophenyl)ethyl]-methyl-amide

HRID 1351301노트

반응식

HRID 1351301 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][N:10]([CH3:21])[S:11]([C:14]2[CH:18]=[C:17]([CH:19]=[O:20])[S:16][CH:15]=2)(=[O:13])=[O:12])=[CH:4][CH:3]=1.[CH:22]([Mg]Br)([CH3:24])[CH3:23].O1CCCC1.[Cl-].[NH4+]>O1CCCC1>[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][N:10]([CH3:21])[S:11]([C:14]2[CH:18]=[C:17]([CH:19]([OH:20])[CH:22]([CH3:24])[CH3:23])[S:16][CH:15]=2)(=[O:13])=[O:12])=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 860714225-Formylthiophene-3-sulfonic acid [2-(4-fluorophenyl)ethyl]-methyl-amideHCID 178420663HCID 178420663, 화합물

생성물 1

HCID 866009945-(1-Hydroxy-2-methylpropyl)thiophene-3-sulfonic acid [2-(4-fluorophenyl)ethyl]-methyl-amide

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 5-formylthiophene-3-sulfonic acid [2-(4-fluorophenyl)ethyl]-methyl-amide (138 mg) in tetrahydrofuran (2 mL) was added dropwise a solution (0.25 mL) of 2.0M isopropyl magnesium bromide-tetrahydrofuran on an ice bath. After stirring for 1 hour, an aqueous solution of saturated ammonium chloride was added, and the solution was extracted with ethyl acetate. After drying the organic layer with anhydrous sodium sulfate, the residue that was obtained upon removing the solvent by evaporation was purified by silica gel column chromatography (hexane/ethyl acetate) and the title compound (57 mg) was obtained as a yellow oily substance.

후처리

  1. extractionthe solution was extracted with ethyl acetate
  2. dry with materialAfter drying the organic layer with anhydrous sodium sulfate
  3. customthe residue that was obtained
  4. customupon removing the solvent
  5. customby evaporation
  6. customwas purified by silica gel column chromatography (hexane/ethyl acetate)

출처 및 근거

ORD 기록
ord-96ca926655eb47df8d7ed6a88640f65f
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07217723B2

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