HRID443921

反应详情

EQUATION

反应方程式

HRID 443921 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.6 g of H-MePhe-OH are dissolved in a mixture of ter.-butanol, 25 ml of 10% aqueous KHCO3 solution and 5 ml of 4 N sodium hydroxide. 8 ml of di-tert.-butylcarbonate are added and the mixture stirred for 2 days at room temperature. The reaction mixture is diluted with ca. 100 ml of water and extracted with ether. The aqueous phase is acidified, with stirring to pH 2. The precipitated product is extracted with acetic acid, the extract washed with water and dried over Na2SO4. The liquid is evaporated and the product crystallised from ether/petroleum ether to yield Boc-MePHe-OH. M.P. 87°.

WORKUP

后处理

  1. extractionextracted with ether
  2. stirringwith stirring to pH 2
  3. extractionThe precipitated product is extracted with acetic acid
  4. washthe extract washed with water
  5. dry with materialdried over Na2SO4
  6. customThe liquid is evaporated
  7. customthe product crystallised from ether/petroleum ether