HRID1390669

反应详情

EQUATION

反应方程式

HRID 1390669 的结构方程式

PROCEDURE

实验过程

The pH of the 4-chloro-2-fluorophenylhydrazine hydrochloride slurry was adjusted to 3.8-4.0 and the temperature was raised to 90°-95°. To this mixture was added an aqueous solution (preheated to 90°-95°) of 1118 parts of cyclohexanone-2-carboxamide prepared as previously described. The resulting mixture was heated for 1-2 hr at 90°-95° during which time the product precipitated from solution. The product was isolated by filtration, washed by digestion with toluene and air-dried to give 1771 parts of an indazolone, an off-white solid mp 179-182 which was 2-(4-chloro-2-fluorophenyl)-1,2,4,5,6,7-hexahydro-3H-indazol-3-one.

WORKUP

后处理

  1. temperaturethe temperature was raised to 90°-95°
  2. customprepared
  3. temperatureThe resulting mixture was heated for 1-2 hr at 90°-95° during which time the product
  4. customprecipitated from solution
  5. customThe product was isolated by filtration
  6. washwashed by digestion with toluene
  7. customair-dried