HRID1988263

反应详情

EQUATION

反应方程式

HRID 1988263 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To a solution of Z-Tyr(3-tBu)-H (2.18 g, 6.14 mmol) in ethanol (25 ml), potassium cyanide (480 mg, 7.37 mmol), 30% ammonium carbonate (1.77 g, 18.4 mmol) and water (25 ml) were added and stirred at 60° C. for 8 hours. The mixture was left for cooling and mixed with a saturated aqueous NaHCO3 solution. The organic layer was extracted with ethyl acetate and washed with water and then with saturated brine, dried over anhydrous magnesium sulfate and evaporated to remove the solvent under reduced pressure; the thus obtained residue was subjected to silica gel column chromatography (developing solvent: ethyl acetate:n-hexane=1:1), giving the titled compound (1.38 g, 53%).

WORKUP

后处理

  1. waitThe mixture was left
  2. temperaturefor cooling
  3. extractionThe organic layer was extracted with ethyl acetate
  4. washwashed with water
  5. dry with materialwith saturated brine, dried over anhydrous magnesium sulfate
  6. customevaporated
  7. customto remove the solvent under reduced pressure