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Methanesulfonic Acid → Methyl(7-fluoro-6-methoxy-4-methyl-1-benzothiophen-3-yl)acetate

HRID 591445
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인쇄 미리보기

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HRID 591445 반응식
S(O)(C)(=O)=O.[F:6][C:7]1[C:12]([O:13][CH3:14])=[CH:11][C:10]([CH3:15])=[CH:9][C:8]=1[S:16][CH2:17][C:18](=O)[CH2:19][C:20]([O:22][CH3:23])=[O:21]>>[CH3:23][O:22][C:20](=[O:21])[CH2:19][C:18]1[C:9]2[C:10]([CH3:15])=[CH:11][C:12]([O:13][CH3:14])=[C:7]([F:6])[C:8]=2[S:16][CH:17]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 6395Methanesulfonic AcidHCID 89767691Methyl 4-((2-fluoro-3-methoxy-5-methylphenyl)sulfanyl)-3-oxobutanoate

생성물 1

HCID 121004334Methyl(7-fluoro-6-methoxy-4-methyl-1-benzothiophen-3-yl)acetate수율 96.7%

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온도
0 °C

실험 절차

MsOH (3.0 mL) was added to methyl 4-((2-fluoro-3-methoxy-5-methylphenyl)sulfanyl)-3-oxobutanoate (330 mg) at 0° C. After stirring at 0° C. for 10 min, the mixture was poured into ice water at 0° C. and extracted with EtOAc. The organic layer was separated, washed successively with saturated aqueous NaHCO3 and brine, dried over MgSO4 and concentrated in vacuo. The residue was purified by silica gel column chromatography (EtOAc/hexane) to give the title compound (299 mg).

후처리

  1. extractionextracted with EtOAc
  2. customThe organic layer was separated
  3. washwashed successively with saturated aqueous NaHCO3 and brine
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified by silica gel column chromatography (EtOAc/hexane)

출처 및 근거

ORD 기록
ord-789bd90cd1ab4c93935abce7daa84cf8
출처 데이터셋
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09238639B2

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