HRID1253098
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
960 mg of H-Ala-Sta-OMe, 1 g of Boc-Sta-OH, 420 mg of HONSu and 750 mg of DCCI are dissolved successively in 50 ml of CH2Cl2 at RT. A white precipitate appears very quickly. The mixture is stirred at RT and, after 7 h, the DCU formed is filtered off and washed with CH2Cl2. The organic solution is washed successively with KHSO4 --K2SO4 (5% solution in H2O) and NaHCO3 (5% solution in H2O). It is dried over MgSO4 and filtered and the solvent is evaporated off. The product is solubilized in the minimum quantity of a chloroform/MeOH mixture (97.5/2.5, vol/vol) and deposited on the top of a column of silica gel; elution is carried out with the same mixture and the eluate is fractionated.
WORKUP
后处理
- customthe DCU formed
- filtrationis filtered off
- washwashed with CH2Cl2
- washThe organic solution is washed successively with KHSO4
- dry with materialIt is dried over MgSO4
- filtrationfiltered
- customthe solvent is evaporated off
- washelution