4-Ethylaniline → 4-Ethyl-3-nitroaniline

HRID 40462

반응식

HRID 40462 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° C. 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° C. 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-69c73ab94c674bf8a16462da5a44413a
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08530388B2

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