HRID1890398

反应详情

EQUATION

反应方程式

HRID 1890398 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of 0.100 g (0.30 mmol) of (+/−)-9-amino-4-oxo-2-pyrimidin-4-yl-5,6,8,9-tetrahydro-4H-1,4a,7-triaza-benzocycloheptene-7-carboxylic acid ethyl ester dissolved in 1.50 mL of dimethylformamide was added 0.041 g (0.33 mmol) of 2-pyridine carboxylic acid. To the resulting mixture was added 50 μL (0.33 mmol) of diethyl cyanophosphonate and 130 μL (0.91 mmol) of triethylamine at 0° C. The resulting mixture was stirred at room temperature for 15 hours. Water and ethyl acetate were added and the mixture was stirred. The resulting residue was filtered, washed with water, ethyl acetate and diethyl ether to afford 0.098 g (76%) of the pure product as a white powder.

WORKUP

后处理

  1. stirringthe mixture was stirred
  2. filtrationThe resulting residue was filtered
  3. washwashed with water, ethyl acetate and diethyl ether