Methanol → HCID 60451708, 화합물

HRID 417303노트

반응식

HRID 417303 반응식
[CH2:1]([O:5][C:6]1[CH:7]=[C:8]([CH:12]=[CH:13][C:14]=1[N+:15]([O-:17])=[O:16])[C:9]([OH:11])=[O:10])[CH2:2][CH2:3][CH3:4].OS(O)(=O)=O.[CH3:23]O>>[CH2:1]([O:5][C:6]1[CH:7]=[C:8]([CH:12]=[CH:13][C:14]=1[N+:15]([O-:17])=[O:16])[C:9]([O:11][CH3:23])=[O:10])[CH2:2][CH2:3][CH3:4]

참가 물질

4

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 2535313-Butoxy-4-nitrobenzoic acid

생성물 1

HCID 60451708HCID 60451708, 화합물수율 95%

실험 절차

To a solution of 3-butoxy-4-nitrobenzoic acid (City Chemicals) (2.5 g, 10.5 mmol) in methanol (10 mL) were added concentrated H2SO4 (1 g, 10.5 mmol). The reaction mixture was heated at reluxing for 2 h. The mixture was concentrated. The residue was partitioned between ethyl acetate and water. The organic layer was separated, and aqueous layer was extracted with ethyl acetate twice. The combined organic extract was washed with water, aqueous saturated NaHCO3 solution, brine, dried over MgSO4, and concentrated to give methyl 3-butoxy-4-nitrobenzoate as a brown oil (2.5 g, 95%).

후처리

  1. temperatureThe reaction mixture was heated
  2. concentrationThe mixture was concentrated
  3. customThe residue was partitioned between ethyl acetate and water
  4. customThe organic layer was separated
  5. extractionaqueous layer was extracted with ethyl acetate twice
  6. extractionThe combined organic extract
  7. washwas washed with water, aqueous saturated NaHCO3 solution, brine
  8. dry with materialdried over MgSO4
  9. concentrationconcentrated

출처 및 근거

ORD 기록
ord-3aeefc76e4004d3997b01eafcac4050b
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08088815B2

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