HRID1252621
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
To a suspension of 4,5-bis(phenylmethoxy)-2-pyridinecarboxylic acid (7.1 g, 21.17 mmol), hydroxybenzotriazole (0.29 g, 2.12 mmol) and N-aminopiperazine-2,3-dione (2.73 g, 21.17 mmol) in 140 ml of dry dimethylformamide was added, after 15 minutes of stirring, 4.80 g (23.3 mmol) of dicyclohexylcarbodiimide. After stirring for 21 hours at room temperature, dicyclohexylurea was filtered off (4.0 g ) and the solvent was evaporated in vacuo. The solid residue was triturated for 40 minutes with 240 ml of tetrahydrofuran, filtered, washed with tetrahyrofuran and dried in vacuo to yield 7.76 g of the title compound, melting point 231.1° C.
WORKUP
后处理
- additionwas added, after 15 minutes
- stirringAfter stirring for 21 hours at room temperature
- filtrationdicyclohexylurea was filtered off (4.0 g )
- customthe solvent was evaporated in vacuo
- customThe solid residue was triturated for 40 minutes with 240 ml of tetrahydrofuran
- filtrationfiltered
- washwashed with tetrahyrofuran
- customdried in vacuo