HRID1979636

反应详情

EQUATION

反应方程式

HRID 1979636 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

Following a procedure of P. Brookes, et al., J. Chem. Soc., 3165 (1957), 1-benzyl-4-piperidinone (44.6 g, 0.234 mol) and hydroxylamine hydrochloride (14.0 g, 0.201 mol) are added to 140 ml of dry pyridine and the resulting mixture is heated to 100° C. in an oil bath for 3 hours. The resulting solid is cooled overnight, filtered and crystallized from 1 liter of ethanol. The product is collected as colorless needles, 38.17 g, in two groups with melting point of 225°-237° C., decomposed depending upon the rate of heating.

WORKUP

后处理

  1. temperatureThe resulting solid is cooled overnight
  2. filtrationfiltered
  3. customcrystallized from 1 liter of ethanol
  4. customThe product is collected as colorless needles, 38.17 g, in two groups with melting point of 225°-237° C.
  5. temperatureof heating