4-Ethylaniline → 4-Ethyl-3-nitroaniline

HRID 72248

반응식

HRID 72248 반응식
[N+:1]([O-:4])([O-])=[O:2].[NH4+].[CH2:6]([C:8]1[CH:14]=[CH:13][C:11]([NH2:12])=[CH:10][CH:9]=1)[CH3:7]>S(=O)(=O)(O)O>[CH2:6]([C:8]1[CH:14]=[CH:13][C:11]([NH2:12])=[CH:10][C:9]=1[N+:1]([O-:4])=[O:2])[CH3:7]

참가 물질

4

반응물 2

HCID 115044-EthylanilineHCID 22985Ammonium nitrate

생성물 1

HCID 227086804-Ethyl-3-nitroaniline수율 75.2%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

Ammonium nitrate (39.6 g, 0.49 mol) is added portionwise to a chilled (ice-bath) solution of 4-ethylaniline (20 g, 0.16 mol) in concentrated sulfuric acid (100 ml), maintaining the temperature at −10° to 0° C. by external cooling. The reaction mixture is stirred for two hours, then poured onto crushed ice, and the precipitate is collected by filtration. The solid is taken up in water, the solution made neutral by addition of dilute aqueous sodium hydroxide solution and extracted with ethyl acetate. The organic extracts are combined, dried over anhydrous sodium sulfate, filtered and the filtrate is evaporated in vacuo to give 4-ethyl-3-nitroaniline (20 g).

후처리

  1. temperaturemaintaining the temperature at −10° to 0° C. by external cooling
  2. additionpoured
  3. customonto crushed ice
  4. filtrationthe precipitate is collected by filtration
  5. additionthe solution made neutral by addition of dilute aqueous sodium hydroxide solution
  6. extractionextracted with ethyl acetate
  7. dry with materialdried over anhydrous sodium sulfate
  8. filtrationfiltered
  9. customthe filtrate is evaporated in vacuo

출처 및 근거

ORD 기록
ord-ccbe8c60394f48e99f50168cdb926c5d
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08828908B2

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