HRID1155537

反应详情

EQUATION

反应方程式

HRID 1155537 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of 3.1 g. (45 mmoles) of hydroxylamine hydrochloride in 10 ml. of water was added 22.5 ml. of 2 N sodium hyroxide solution. To this solution was added 3.6 g. (26 mmoles) of 1-(2-amino-4-pyridyl)-1-ethanone and the mixture heated to the boiling point for 5 minutes. Methanol was added slowly until the mixture became homogeneous. Heating was continued until a precipitate began to form. The mixture was cooled to 0° C., and the resulting precipitate was filtered, washed with water and dried in vacuo. Recrystallization from ethyl acetate afforded 3.6 g. (92%) of the desired oxime, m.p. 215°-217° C.

WORKUP

后处理

  1. additionTo this solution was added 3.6 g
  2. temperatureHeating
  3. customto form
  4. filtrationthe resulting precipitate was filtered
  5. washwashed with water
  6. customdried in vacuo
  7. customRecrystallization from ethyl acetate
  8. customafforded 3.6 g