Water → 2,4-Dimethyl-5-nitroaniline

HRID 618223

반응식

HRID 618223 반응식
[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[C:5]([N+:9]([O-:11])=[O:10])=[CH:4][C:3]=1[NH:12]C(=O)C.O.S(=O)(=O)(O)O>C(O)C>[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[C:5]([N+:9]([O-:11])=[O:10])=[CH:4][C:3]=1[NH2:12]

참가 물질

5

반응물 3

HCID 962WaterHCID 1118Sulfuric AcidHCID 112848Acetamide, N-(2,4-dimethyl-5-nitrophenyl)-

생성물 1

HCID 2280072,4-Dimethyl-5-nitroaniline

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of N-(2,4-dimethyl-5-nitrophenyl)acetamide, water (24 mL), concentrated sulfuric acid (12 mL), and ethanol (120 mL) was heated at reflux under an atmosphere of nitrogen for 4 hours. The ethanol was evaporated under reduced pressure and the residue partitioned between ethyl acetate (250 mL) and brine (150 mL). The brine solution was reextracted with ethyl acetate. The combined ethyl acetate extracts were then dried over magnesium sulfate. Evaporation afforded a crude product which was flash chromatographed on silica and eluted with ethyl acetate:hexane (1:4) to afford 4.63 g as a pale yellow solid.

후처리

  1. temperaturewas heated
  2. temperatureat reflux under an atmosphere of nitrogen for 4 hours
  3. customThe ethanol was evaporated under reduced pressure
  4. customthe residue partitioned between ethyl acetate (250 mL) and brine (150 mL)
  5. dry with materialThe combined ethyl acetate extracts were then dried over magnesium sulfate
  6. customEvaporation

출처 및 근거

ORD 기록
ord-4de117abeb1f4784a6bf1ac634204bc3
출처 데이터셋
uspto-grants-1999_09
특허 번호
US05952362

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