Methanol → Methyl 4-nitroanthranilate

HRID 581661

반응식

HRID 581661 반응식
[NH2:1][C:2]1[CH:10]=[C:9]([N+:11]([O-:13])=[O:12])[CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].S(=O)(=O)(O)O.[CH3:19]O>>[NH2:1][C:2]1[CH:10]=[C:9]([N+:11]([O-:13])=[O:12])[CH:8]=[CH:7][C:3]=1[C:4]([O:6][CH3:19])=[O:5]

참가 물질

4

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 120764-Nitroanthranilic acid

생성물 1

HCID 596476Methyl 4-nitroanthranilate수율 89%

실험 절차

A mixture of 118.8 g of 2-amino-4-nitro-benzoic acid, 1000 ml of methanol and 120 ml of concentrated sulfuric acid is heated at the boiling point for 16 hours. The mixture is concentrated under reduced pressure, the residue is taken up in ethyl acetate and the mixture is washed with saturated NaHCO3 solution. After drying over Na2SO4, the organic phase is concentrated. 114.2 g (89%) of methyl 2-amino-4-nitro-benzoate are thus obtained with a melting point (m.p.) of 156-158° C.

후처리

  1. temperatureis heated at the boiling point for 16 hours
  2. concentrationThe mixture is concentrated under reduced pressure
  3. washthe mixture is washed with saturated NaHCO3 solution
  4. dry with materialAfter drying over Na2SO4
  5. concentrationthe organic phase is concentrated

출처 및 근거

ORD 기록
ord-4f8c35cb17de4c0ca3cb4158075d7987
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05922646

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