HRID1492398
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of 62.5 g of 6-(4,4-ethylenedioxy-1-piperidinyl)-8-methyl-1,2,4-triazolo [4,3-b]pyridazine in 350 ml of aqueous 10% acetic acid was refluxed for 7 hours. The solvent was then evaporated under reduced pressure and the residue was taken up in 1100 ml of boiling ethanol. The ethanol solution was concentrated to 600 ml and cooled in an ice bath. The crystalline solid which formed was separated by filtration, washed with fresh ethanol and then with ethyl ether and dried to give 1-(8-methyl-1,2,4-triazolo [4,3-b]pyridazin-6-yl)-4-piperidinone as cream-colored needles melting at about 196.5°-199° C.
WORKUP
后处理
- customThe solvent was then evaporated under reduced pressure
- concentrationThe ethanol solution was concentrated to 600 ml
- temperaturecooled in an ice bath
- customThe crystalline solid which formed
- customwas separated by filtration
- washwashed with fresh ethanol
- dry with materialwith ethyl ether and dried