HRID1870671

反应详情

EQUATION

反应方程式

HRID 1870671 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 17.3 g (0.1 mol) of 5-amino-3-methyl-1-phenylpyrazole in 200 cm3 of absolute ethanol were added dropwise 0.5 cm3 of 12N hydrochloric acid and then 13.5 cm3 of isoamyl nitrite, at 0° C. The solution was then warmed to and left at room temperature for 4 hours. An orange-coloured solid crystallized out. This solid was filtered off on a sinter funnel and washed with 100 cm3 of isopropyl ether. After drying under vacuum at room temperature, 17 g of 5-amino-3-methyl-4-nitroso-1-phenylpyrazole were obtained in the form of an orange-coloured solid, the melting point of which was from 202 to 204° C.

WORKUP

后处理

  1. customat 0° C
  2. temperatureThe solution was then warmed to and
  3. customAn orange-coloured solid crystallized out
  4. filtrationThis solid was filtered off on a sinter funnel
  5. washwashed with 100 cm3 of isopropyl ether
  6. customAfter drying under vacuum at room temperature