HRID275733

反应详情

EQUATION

反应方程式

HRID 275733 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1.83 g of 6,7-dimethoxy-2-methylamino-4-(3-nitrophenyl) quinazoline obtained in Production Example 4,200 mg of 10% palladium-carbon powder (hydrate) and 1.44 g triethylamine were suspended in a mixed solvent of 10 ml ethanol and 10 ml tetrahydrofuran. After the atmosphere was replaced with hydrogen, the mixture was stirred for 15 hours at ordinary pressure at room temperature. The reaction solution was filtered, then the filtrate was evaporated, and the crude product was purified and separated by silica gel column chromatography (hexane:ethyl acetate=1:3). The product was recrystallized from hexane-ethyl acetate to give 1.22 g of the title compound as pale yellow crystals.

WORKUP

后处理

  1. filtrationThe reaction solution was filtered
  2. customthe filtrate was evaporated
  3. customthe crude product was purified
  4. customseparated by silica gel column chromatography (hexane:ethyl acetate=1:3)
  5. customThe product was recrystallized from hexane-ethyl acetate