Hydrochloric Acid → 2-Amino-5-(diethylamino)toluene

HRID 1632329

反応式

HRID 1632329 の反応式
[CH2:1]([N:3]([CH2:11][CH3:12])[C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([CH3:10])[CH:5]=1)[CH3:2].Cl.[N:14](OC)=[O:15]>O>[CH2:11]([N:3]([CH2:1][CH3:2])[C:4]1[CH:9]=[CH:8][C:7]([NH2:14])=[C:6]([CH3:10])[CH:5]=1)[CH3:12].[CH2:11]([N:3]([CH2:1][CH3:2])[C:4]1[CH:9]=[CH:8][C:7]([N:14]=[O:15])=[C:6]([CH3:10])[CH:5]=1)[CH3:12]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 12231Methyl nitrite2 回HCID 66679N,N-diethyl-m-toluidine

生成物 2

HCID 673642-Amino-5-(diethylamino)tolueneHCID 80921Benzenamine, N,N-diethyl-3-methyl-4-nitroso-

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

81.5 g of N,N-diethyl-m-toluidine is initially introduced into a stirred flask with 46 ml of hydrochloric acid in 400 ml of water, the reaction mixture is cooled to 0° and gaseous methyl nitrite is passed in, while stirring and cooling. When the introduction of methyl nitrite has ended, the reaction mixture is brought to room temperature, the excess of nitrite is removed in the customary manner by adding urea and the residual gases are removed by applying reduced pressure. The entire reaction mixture is then passed to the catalytic hydrogenation to give 4N,4N-diethyl-2-methyl-p-phenylenediamine without the N,N-diethyl-3-methyl-4-nitroso-aniline formed being isolated. When the hydrogenation has ended, 4N,4N-diethyl-2-methyl-p-phenylenediamine hydrochloride is isolated by precipitation with ethanol. M.p. 268°-272°.

後処理

  1. temperaturethe reaction mixture is cooled to 0°
  2. temperaturecooling
  3. customis brought to room temperature
  4. customthe excess of nitrite is removed in the customary manner
  5. additionby adding urea
  6. customthe residual gases are removed
  7. customThe entire reaction mixture

出典と根拠

ORDレコード
ord-bb35a2705c754764bb9570df858876e3
出典データセット
uspto-grants-1984_10
特許番号
US04474987

関連ノート

読み込み中…