Methanol → Methyl 3-hydroxy-4-nitrobenzoate

HRID 241321

반응식

HRID 241321 반응식
[OH:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[N+:11]([O-:13])=[O:12])[C:5]([OH:7])=[O:6].OS(O)(=O)=O.[CH3:19]O>>[CH3:19][O:6][C:5](=[O:7])[C:4]1[CH:8]=[CH:9][C:10]([N+:11]([O-:13])=[O:12])=[C:2]([OH:1])[CH:3]=1

참가 물질

4

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 692653-Hydroxy-4-nitrobenzoic acid

생성물 1

HCID 294866Methyl 3-hydroxy-4-nitrobenzoate

반응 조건

온도
60 °C

실험 절차

3-Hydroxy-4-nitro-benzoic acid (10 g) was dissolved in MeOH (500 ml). 96% H2SO4 (2 ml) was added, and the mixture was heated to 60° C. for 18 hours. The reaction mixture was concentrated to approx. 200 ml, diluted with EtOAc (200 ml) and washed with an aqueous saturated solution of NaHCO3 (2×20 ml). The organic layer was dried over Na2SO4 and the solvent was removed by evaporation to yield 10.5 g of the desired intermediate.

후처리

  1. concentrationThe reaction mixture was concentrated to approx. 200 ml
  2. additiondiluted with EtOAc (200 ml)
  3. washwashed with an aqueous saturated solution of NaHCO3 (2×20 ml)
  4. dry with materialThe organic layer was dried over Na2SO4
  5. customthe solvent was removed by evaporation

출처 및 근거

ORD 기록
ord-e14db1b97e2d4dc3bb7866cd1557f075
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08648204B2

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