HRID519415

反应详情

EQUATION

反应方程式

HRID 519415 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Water (2 ml) was added to a solution of Boc-Arg-OH (2.5 mmol) in methanol (20 ml). The solution was neutralised with a 20% solution of Cs2CO3 in water and then evaporated in vacuo to dryness. Residual water was removed by repeated addition and evaporation of toluene. The solid cesium salt of Boc-arginine was treated with DMF (25 ml) and benzyl bromide (3 mmol) and stirred at room temperature for 6 h. The DMF was removed in vacuo and the product was dissolved in acetone and filtered. The filtrate was evaporated in vacuo and the product was treated with 95% trifluoroactetic acid (TFA) (4 ml). The resulting product H-Arg-OBzl was isolated by tituration by diethyl ether. The salt of H-Arg-OBzl was isolated by treating the product with para-toluenesulfonic acid (5 mmol) in ether.

WORKUP

后处理

  1. customevaporated in vacuo to dryness
  2. customResidual water was removed
  3. additionaddition and evaporation of toluene
  4. customThe DMF was removed in vacuo
  5. dissolutionthe product was dissolved in acetone
  6. filtrationfiltered
  7. customThe filtrate was evaporated in vacuo
  8. additionthe product was treated with 95% trifluoroactetic acid (TFA) (4 ml)