HRID617956

反应详情

EQUATION

反应方程式

HRID 617956 的结构方程式

PROCEDURE

实验过程

6-(2,6-Dibromo-phenyl)-N2 -[3-diethylamino-propyl)-pyrido[2,3-d]pyrimidine-2,7-diamine (0.34 g) from Example 61 was reacted with 0.066 g of tert-butyl isocyanate according to the general procedure of Example 54. The crude residue was purified by thin layer chromatography with ethyl acetate:ethanol:triethylamine (9:2:1) followed by preparative HPLC chromatography using a Vydac 218 TP 1022 reverse phase column with a gradient elution of 0.1% trifluoroacetic acid/water and 0.1% trifluoroacetic acid/acetonitrile to give 0.214 g of the title compound, ESMS (20/80 MEOH/CH3CN+0.1% AcOH): 606=M+ +H; mp dec. >45° C.

WORKUP

后处理

  1. customThe crude residue was purified by thin layer chromatography with ethyl acetate:ethanol:triethylamine (9:2:1)
  2. washwith a gradient elution of 0.1% trifluoroacetic acid/water and 0.1% trifluoroacetic acid/acetonitrile