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
Into a mixture of 0.3 g (1.28×10-3 mol) of 1-methylpropyl-5-[4-hydroxyphenyl]-1,3,4-thiadiazole, 0.26 g (1.31×10-3 mol) of trans-4-n-pentylcyclohexanecarboxylic acid, 0.27 g (1.31×10-3 mol) of dicyclohexylcarbodiimide and 0.03 g of 4-(1-pyrrolidinyl)pyrimidine, 15 ml of methylene chloride was added, followed by 20 hours of stirring at room temperature. After the reaction, the reaction was filtered and the solid was washed with methylene chloride. The filtrate and the washing liquid were dehydrated, and the solvent was distilled off therefrom to obtain a crude product, which was then recrystallized twice to obtain 0.24 g of 2-(1-methylpropyl)-5-[4-(trans-4-n-pentylcyclohexylcarbonyloxy)-phenyl]-1,3,4-thiadiazole. (Yield: 45.2%).
WORKUP
后处理
- additionwas added
- customAfter the reaction
- filtrationthe reaction was filtered
- washthe solid was washed with methylene chloride
- distillationthe solvent was distilled off
- customto obtain a crude product, which
- customwas then recrystallized twice