HRID1155541

反应详情

EQUATION

反应方程式

HRID 1155541 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 7 g. (0.1 mole) of hydroxylamine hydrochloride in 40 ml. of water and 50 ml. of 2 N sodium hydroxide was added 11.5 g. (70 mmoles) of 1-(2-ethylamino-4-pyridyl)-1-ethanone, and the resulting mixture heated to boiling. Methanol was carefully added until the mixture became homogeneous. Heating was continued until the mixture became cloudy. The mixture was cooled and the resulting precipitate filtered, washed with water and dried. Recrystallization from toluene gave 10.9 g. (87%) of the desired product, m.p. 155°-156° C.

WORKUP

后处理

  1. additionTo a mixture of 7 g
  2. temperatureHeating
  3. temperatureThe mixture was cooled
  4. filtrationthe resulting precipitate filtered
  5. washwashed with water
  6. customdried
  7. customRecrystallization from toluene
  8. customgave 10.9 g