HRID1952756
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 mixture of 1-(1,4-benzodioxan-5-yl)piperazine (1 g; prepared in a similar manner to that described in Example 2), 4-allyl-5-(3-pyridyl)-1,2,4-triazole-3(2H,4H)-thione (1 g), 37-40% aqueous formaldehyde solution (0.5 ml) and t-butanol (60 ml) was stirred at ambient temperature for 30 minutes, heated under reflux for 15 minutes, then the solvent was removed in vacuo. The residue was triturated with a 1:1 mixture of cyclohexane and ether (40 ml), and the resulting solid was collected by filtration and dried in vacuo at ambient temperature to give 4-allyl-2-[4-(1,4-benzodioxan-5-yl)piperazin-1-ylmethyl]-5-(3-pyridyl)-1,2,4-triazole-3(2H,4H)-thione as a white solid (0.62 g), m.p. 122-127° C.
WORKUP
后处理
- customprepared in a similar manner to that
- temperatureheated
- temperatureunder reflux for 15 minutes
- customthe solvent was removed in vacuo
- customThe residue was triturated with a 1:1 mixture of cyclohexane and ether (40 ml)
- filtrationthe resulting solid was collected by filtration
- customdried in vacuo at ambient temperature