Acetic Acid → 4-Amino-2-fluoro-3-methoxybenzoic acid

HRID 1880974노트

반응식

HRID 1880974 반응식
[F:1][C:2]1[C:9]([O:10][CH3:11])=[C:8]([N+:12]([O-])=O)[CH:7]=[CH:6]C=1C#N.[H][H].[C:17]([OH:20])(=[O:19])[CH3:18]>OS(O)(=O)=O.O.CO>[NH2:12][C:8]1[CH:7]=[CH:6][C:18]([C:17]([OH:20])=[O:19])=[C:2]([F:1])[C:9]=1[O:10][CH3:11]

참가 물질

7

반응물 3

HCID 176Acetic AcidHCID 579555492-Fluoro-3-methoxy-4-nitrobenzonitrileHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 193583414-Amino-2-fluoro-3-methoxybenzoic acid

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 1118Sulfuric Acid용매

실험 절차

A solution of 2-fluoro-3-methoxy-4-nitrobenzonitrile (170 mg) in H2SO4 and H2O (0.5 mL/0.5 mL) was heated at 100° C. for 18 h. After which, it was separated between ethyl acetate and water. Organic extract was dried and concentrated to give a residue, which was then dissolved in a mixture of methanol and acetic acid (2 mL/2 mL) and was hydrogenated using hydrogen balloon overnight. The solution was filtered through celite, and the filtrate concentrated to give a read solid as the product. [M+H] calc'd for C8H8FNO3, 186; found 186.

후처리

  1. customAfter which, it was separated between ethyl acetate and water
  2. extractionOrganic extract
  3. customwas dried
  4. concentrationconcentrated
  5. customto give a residue, which
  6. filtrationThe solution was filtered through celite
  7. concentrationthe filtrate concentrated
  8. customto give a read solid as the product

출처 및 근거

ORD 기록
ord-769799971bf84eeea1706a67bb5eb0f4
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08318727B2

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