HRID127004

反应详情

EQUATION

反应方程式

HRID 127004 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1.19 g (5.00 m moles) L-3-(3,4-dihydroxyphenyl)-2-methylalanine, 1.49 g (5.00 m moles) t-butyl 2,4,5-trichlorophenylcarbonate and 6 ml dimethylformamide is flushed with nitrogen and 1.39 ml (10.0 m moles) triethylamine is added. After stirring at room temperature for 24 hours, 60 ml H2O and 4 ml 2.5 N HCl is added. The solution is extracted 3 times with 50 ml of ethyl acetate and the extract is washed 3 times with 50 ml of water and 1 time with 50 ml of saturated sodium chloride solution and is dried (MgSO4). The solvent is removed in vacuum to give 1.98 g of a blue oil.

WORKUP

后处理

  1. customis flushed with nitrogen and 1.39 ml (10.0 m moles) triethylamine
  2. additionis added
  3. addition60 ml H2O and 4 ml 2.5 N HCl is added
  4. extractionThe solution is extracted 3 times with 50 ml of ethyl acetate
  5. washthe extract is washed 3 times with 50 ml of water and 1 time with 50 ml of saturated sodium chloride solution
  6. dry with materialis dried (MgSO4)
  7. customThe solvent is removed in vacuum