HRID1632329

反应详情

EQUATION

反应方程式

HRID 1632329 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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°.

WORKUP

后处理

  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