Ethanol → Ethyl 4-fluoro-3-nitrobenzoate

HRID 40112

반응식

HRID 40112 반응식
[F:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][C:3]=1[N+:11]([O-:13])=[O:12].OS(O)(=O)=O.C([O-])(O)=O.[Na+].[O-]S([O-])(=O)=O.[Mg+2].[CH3:30][CH2:31]O>>[F:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([O:8][CH2:30][CH3:31])=[O:7])=[CH:4][C:3]=1[N+:11]([O-:13])=[O:12]

참가 물질

6

반응물 5

HCID 702EthanolHCID 1118Sulfuric AcidHCID 24083Sulfuric acid magnesium salt (1:1)HCID 679874-Fluoro-3-nitrobenzoic acidHCID 516892Sodium Bicarbonate

생성물 1

HCID 21277355Ethyl 4-fluoro-3-nitrobenzoate

반응 조건

온도
0 °C

실험 절차

A solution of 4-fluoro-3-nitrobenzoic acid (Alfa Aesar, 10.0 g, 54 mmol) and concentrated H2SO4 (0.2 ml, 4.1 mmol) in EtOH (200 ml) was refluxed for 40 h. The mixture was cooled to 0° C., solid NaHCO3 and MgSO4 was added, and the suspension was filtered and concentrated in vacuo. The residue was purified by chromatography on silica gel (0→30% EtOAc-hexanes) to yield the title compound as an off-white solid.

후처리

  1. filtrationthe suspension was filtered
  2. concentrationconcentrated in vacuo
  3. customThe residue was purified by chromatography on silica gel (0→30% EtOAc-hexanes)

출처 및 근거

ORD 기록
ord-c474b033b567489bbfa0e0a712e1b26f
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08524917B2

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