HRID1111721

反应详情

EQUATION

反应方程式

HRID 1111721 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of 9.9 grams of Z-D-Glu-OBzl and 3.6 grams of 1-hydroxybenzotriazole in 50 ml of absolute tetrahydrofurane are added 1.96 grams of tert.-butylamine and at 0° C. 5.86 grams of DCC. The mixture is stirred for 2 hours at 0° C. and overnight at room temperature. The next day the precipitate is filtered off with suction and the filtrate is concentrated. The residue is dissolved in ethyl acetate and the solution is washed in succession with a saturated solution of sodium bicarbonate, 2n-HCl, a saturated solution of sodium bicarbonate and water, dried with sodium sulphate and concentrated. Yield: 4.6 gams of an oil.

WORKUP

后处理

  1. customat 0° C
  2. filtrationThe next day the precipitate is filtered off with suction
  3. concentrationthe filtrate is concentrated
  4. dissolutionThe residue is dissolved in ethyl acetate
  5. washthe solution is washed in succession with a saturated solution of sodium bicarbonate, 2n-HCl
  6. dry with materiala saturated solution of sodium bicarbonate and water, dried with sodium sulphate
  7. concentrationconcentrated