Acetic Acid → 4-Bromo-N-methyl-2-nitroaniline

HRID 420468

반응식

HRID 420468 반응식
C(O)(=O)C.[CH3:5][NH:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[N+:13]([O-:15])=[O:14].[Br:16]N1C(=O)CCC1=O>O>[Br:16][C:10]1[CH:11]=[CH:12][C:7]([NH:6][CH3:5])=[C:8]([N+:13]([O-:15])=[O:14])[CH:9]=1

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 67184N-bromobutanimideHCID 69157Benzenamine, N-methyl-2-nitro-

생성물 1

HCID 2580424-Bromo-N-methyl-2-nitroaniline수율 93.1%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Pouring 60 milliliter of acetic acid over 5.0 g (33 mmol) of N-methyl-2-nitroaniline and 5.9 g (33 mmol) of N-bromosuccinimide, the resultant solution was refluxed with heating for 7 hours. After completion of the reaction, the reacted solution was poured into 500 milliliter of water, and precipitated solids were separated with filtration. Dissolving the resultant solids into ethyl acetate, the resultant solution was dried with the use of magnesium sulfate. After filtration, the solvent was removed by distillation under reduced pressure, and after drying the solids under reduced pressure at room temperature, 7.1 g of 4-bromo-N-methyl-2-nitroaniline as orange solids were obtained (yield: 93%).

후처리

  1. temperaturewith heating for 7 hours
  2. customAfter completion of the reaction
  3. customprecipitated solids
  4. customwere separated with filtration
  5. dissolutionDissolving the resultant solids into ethyl acetate
  6. dry with materialthe resultant solution was dried with the use of magnesium sulfate
  7. filtrationAfter filtration
  8. customthe solvent was removed by distillation under reduced pressure
  9. customafter drying the solids under reduced pressure at room temperature

출처 및 근거

ORD 기록
ord-f90601c1bdb344d6b84112a3453fbf50
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08097349B2

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