4-Ethylaniline → 4-Ethyl-3-nitroaniline

HRID 40462

反応式

HRID 40462 の反応式
[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]

参加物

4

反応物 2

HCID 115044-EthylanilineHCID 22985Ammonium nitrate

生成物 1

HCID 227086804-Ethyl-3-nitroaniline収率 75.2%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-69c73ab94c674bf8a16462da5a44413a
出典データセット
uspto-grants-2013_09
特許番号
US08530388B2

関連ノート

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