HRID1813886
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
0.5 mmol of piperazine was dissolved in 10 ml of DMF and 1.05 mmol of 1,3 di-p-tolylcarbodiimide was added. After 0.5 h. of stirring at room temperature, a small precipitation was filtered off and washed twice with 1 ml of DMF. The filtrates were collected and kept at room temperature overnight. To the DMF solution, 50 ml of water was added. The precipitated solid was filtered and washed with water. The solid was dissolved in ethyl acetate (20 ml) and 0.2 ml of conc. HCl conc. was added. The product began to precipitate within 15 min. After 1 hour, the precipitate was filtered and washed with ethyl ether. Yield=76%.
WORKUP
后处理
- customa small precipitation
- filtrationwas filtered off
- washwashed twice with 1 ml of DMF
- customThe filtrates were collected
- waitkept at room temperature overnight
- additionTo the DMF solution, 50 ml of water was added
- filtrationThe precipitated solid was filtered
- washwashed with water
- dissolutionThe solid was dissolved in ethyl acetate (20 ml)
- addition0.2 ml of conc. HCl conc. was added
- customto precipitate within 15 min
- waitAfter 1 hour
- filtrationthe precipitate was filtered
- washwashed with ethyl ether