反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
22 g (75 mmol) of 1,4-dibenzyl-2-aminomethylpiperazine dissolved in 300 ml of toluene are mixed with 100 ml of triethylamine in a ground-necked conical flask. 97 ml (0.1 mol) of isopropyl chloroformate, taken up by syringe, are dissolved in 50 ml of toluene, and are then added dropwise to the above solution. At the end of the addition, the mixture is stirred for 2 hours at room temperature. The solution is diluted with ether, washed with saturated NaHCO3 solution and then with water to obtain a neutral pH. The organic phase is dried (MgSO4), filtered and evaporated to give 28.3 g of 1,4-dibenzyl-2-isopropyloxycarbonylaminomethylpiperazine in the form of a viscous compound. Yield: 99.6%. Rf=0.4 (95/5 v/v CH2Cl2/MeOH).
WORKUP
后处理
- additionare then added dropwise to the above solution
- additionAt the end of the addition
- washwashed with saturated NaHCO3 solution
- customwith water to obtain a neutral pH
- dry with materialThe organic phase is dried (MgSO4)
- filtrationfiltered
- customevaporated