HRID2092339

反应详情

EQUATION

反应方程式

HRID 2092339 的结构方程式

CONDITIONS

反应条件

温度
175 °C

PROCEDURE

实验过程

7-(4-Methoxybenzyl)-3-methyl-4-(2-(methylamino)quinazolin-6-yl)-1,7-naphthyridin-8(7H)-one (0.900 g, 2.06 mmol) was taken in a clear microwave vial and treated with 14 ml of TFA and 1 ml of cone HCl. The vial was capped and heated in a Personal Chemistry SmithSynthesizer to 175° C. for 45 minutes. The volatiles were evaporated under reduced pressure and residual TFA/water was azeotroped with toluene. The residue was taken up in DCM/2M MeOH and loaded unto silica. The residue was purified by column chromatography on silica gel using a gradient of 3 to 12% MeOH in DCM to give 3-methyl-4-(2-(methylamino)quinazolin-6-yl)-1,7-naphthyridin-8(7H)-one as a yellow solid. MS(M+H)+ 318.

WORKUP

后处理

  1. customThe vial was capped
  2. customThe volatiles were evaporated under reduced pressure and residual TFA/water
  3. customwas azeotroped with toluene
  4. customThe residue was purified by column chromatography on silica gel using a gradient of 3 to 12% MeOH in DCM