HRID569918

反应详情

EQUATION

反应方程式

HRID 569918 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Hydrazine (0.07 ml) was added dropwise to an ice-cold solution of 0.5 g of 1-benzyl-5,6-dihydro-5-hydroxymethylene-4(1H) cyclopentapyrazolone in 25 ml of methanol. The solution was heated at reflux for 2 hours and then cooled to room temperature and stirred for 16 hours. An additional 0.07 ml of hydrazine was added and the solution was heated at reflux for 8 hours. Removal of the solvent under reduced pressure gave 1-benzyl-4,7-dihydro-1H-cyclopenta-[1,2-c:3,4-c']dipyrazole as an orange-red solid (86% yield) melting at about 61°-72° C.

WORKUP

后处理

  1. temperatureThe solution was heated
  2. temperatureat reflux for 2 hours
  3. temperaturethe solution was heated
  4. temperatureat reflux for 8 hours
  5. customRemoval of the solvent under reduced pressure