HRID2169296

反应详情

EQUATION

反应方程式

HRID 2169296 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 5-benzyloxy-6-hydroxy-2-(1-phenyl-cyclohexylmethyl)-pyrimidine-4-carboxylic acid (2-hydroxyethyl)-isopropylamide (258) (0.43 g, 0.85 mmol) and triphenyl phosphine (0.45 g, 1.71 mmol) in dry dichloromethane (10.0 mL) was added diethyl azidocarboxylate (0.34 mL, 2.13 mmol) at room temperature and the reaction stirred for 2 h. After completion of the reaction, the solvent was evaporated and the crude product was purified by normal silica gel column chromatography (using 2% methanol in dichloromethane) to get 9-benzyloxy-2-isopropyl-6-(1-phenyl-cyclohexylmethyl)-3,4-dihydro-2H-pyrazino[1,2-c]pyrimidine-1,8-dione (259) (0.18 g, 43.0%) as a white solid.

WORKUP

后处理

  1. customAfter completion of the reaction
  2. customthe solvent was evaporated
  3. customthe crude product was purified by normal silica gel column chromatography (using 2% methanol in dichloromethane)