HRID1253098

反应详情

EQUATION

反应方程式

HRID 1253098 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customthe DCU formed
  2. filtrationis filtered off
  3. washwashed with CH2Cl2
  4. washThe organic solution is washed successively with KHSO4
  5. dry with materialIt is dried over MgSO4
  6. filtrationfiltered
  7. customthe solvent is evaporated off
  8. washelution