HRID1730110

反应详情

EQUATION

反应方程式

HRID 1730110 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Two and six-tenths grams (.01 mole) of 2,6-dinitro-4-t-butylchlorobenzene was reacted with 3.1 grams of 40% aqueous solution of methylamine in 50 ml. ethanol. The temperature was slowly increased as follows: 30° C for 1 hour; 40° C for 1 hour; 50° C for 1 hour, then 80° C for 5 hours. When the reaction was complete about 100 ml. H2O was added, precipitating the product. This was filtered, washed with portions of H2O and upon recrystallization from ethanol yielded 2.5 grams of N-methyl-2,6-dinitro-4-t-butylaniline as orange needles melting at 129°-130° C.

WORKUP

后处理

  1. temperatureThe temperature was slowly increased
  2. wait40° C for 1 hour
  3. wait50° C for 1 hour
  4. wait80° C for 5 hours
  5. customprecipitating the product
  6. filtrationThis was filtered
  7. washwashed with portions of H2O and upon recrystallization from ethanol