HRID352387

反应详情

EQUATION

反应方程式

HRID 352387 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 suspension of 7.73 g (50 mmol) of 6-chloropurine in 350 ml of absolute THF were added 14.43 g (55 mmol) triphenylphosphine at −10 to 0° C. followed by 9.57 g (55 mmol) of diethyl azodicarboxylate and 14.8 g (50 mmol) of N-benzyloxycarbonyl-L-serine tert-butyl ester in 100 ml of absolute THF, and the mixture was stirred at 0° C. for 48 h. The solvent was evaporated, the residue was dissolved in EE/heptane (2:1), filtered and the solvent was removed in vacuo. The crude product was purified by flash chromatography on silica gel (EE/n-heptane (1:1) and DCM/EE (85:15)). Yield: 6.6 g.

WORKUP

后处理

  1. customThe solvent was evaporated
  2. dissolutionthe residue was dissolved in EE/heptane (2:1)
  3. filtrationfiltered
  4. customthe solvent was removed in vacuo
  5. customThe crude product was purified by flash chromatography on silica gel (EE/n-heptane (1:1) and DCM/EE (85:15))