HRID1388962

反应详情

EQUATION

反应方程式

HRID 1388962 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Z-Arg-OH.HCl (6 g, 8.7 mmoles) and benzyl mercaptan (4.2 ml, 17.4 mmoles) are dissolved in dimethylformamide (DMF) and cooled to 0° C. DCC (3.6 g, 8.7 mmoles), dissolved in DMF, is then added to the above reaction mixture, stirred at 0° C. for 30 minutes, then stirred overnight at room temperature. The precipitate formed is removed by filtration and the filtrate is concentrated under vacuum to yield an oil. This oily residue is dissolved in ethyl acetate and washed, successively, with 0.1 N HCl, 5% NaHCO3, and saturated aqueous NaCl. The organic layer is dried over anhydrous Na2SO4 and the solvent removed by evaporation. The crude product is purified by silica gel column, using a CHCl3 /methanol system, yielding 4.5 g of the product.

WORKUP

后处理

  1. additionis then added to the above reaction mixture
  2. stirringstirred overnight at room temperature
  3. customThe precipitate formed
  4. customis removed by filtration
  5. concentrationthe filtrate is concentrated under vacuum
  6. customto yield an oil
  7. washwashed
  8. dry with materialThe organic layer is dried over anhydrous Na2SO4
  9. customthe solvent removed by evaporation
  10. customThe crude product is purified by silica gel column