HRID470651

反应详情

EQUATION

反应方程式

HRID 470651 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 1.9 g (27.4 mmol) of hydroxylamine hydrochloride in 22 mL of isopropyl alcohol, 3.3 g (40.3 mmol) of sodium bicarbonate was added. The resulting mixture was stirred at 25° C. to 30° C. for 10-15 min. 2.0 g (18.3 mmol) of cyclohexanecarbonitrile was added and stirred at 80° C. to 85° C. for 3-4 h. After the reaction period, the reaction mass was cooled to 25° C. to 30° C., filtered and washed with 10 mL of isopropyl alcohol. The filtrate was collected and distilled out completely to obtain a crude residue. The residue was chased with 5 mL of toluene, to yield the title compound.

WORKUP

后处理

  1. stirringstirred at 80° C. to 85° C. for 3-4 h
  2. customAfter the reaction period
  3. temperaturethe reaction mass was cooled to 25° C. to 30° C.
  4. filtrationfiltered
  5. washwashed with 10 mL of isopropyl alcohol
  6. customThe filtrate was collected
  7. distillationdistilled out completely
  8. customto obtain a crude residue