HRID2069196

反应详情

EQUATION

反应方程式

HRID 2069196 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To the yellow solution of N-(6-fluoro-7-nitro-2,4-dioxo-1,4-dihydro-2H-quinazolin-3-yl)-methanesulfonamide (500 mg, 1.57 mmol) in ethanol (0.5 ml) is added 2,4-dimethoxybenzylamine (4.72 ml, 31.4 mmol) under argon. The solution is heated at 150° in a closed vial in a microwave reactor for 4 minutes. After removal of the solvent and 2,4-dimethoxybenzylamine by high-vacuum rotavapor evaporation the remaining deep purple oil is treated with diethyl ether to obtain a suspension, which is filtered and dried to yield the crude title compound as a deep purple solid, m.p. 232-237° C.

WORKUP

后处理

  1. temperatureThe solution is heated at 150° in a closed vial in a microwave reactor for 4 minutes
  2. customAfter removal of the solvent and 2,4-dimethoxybenzylamine
  3. customby high-vacuum rotavapor evaporation the remaining deep purple oil
  4. additionis treated with diethyl ether
  5. customto obtain a suspension, which
  6. filtrationis filtered
  7. customdried