HRID127273

反应详情

EQUATION

反应方程式

HRID 127273 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The mixture of 4.79 g of 4-amino-2-chloro-6,7-dimethoxyquinazoline, 4.49 g of 4,4-dimethyl-1-(4-piperidinyl)-piperidin-2,6-dione, 4.24 g of anhydrous sodium carbonate and 75 ml of dimethylformamide is stirred at 150° under nitrogen for 6 hours. It is filtered, the filtrate evaporated, the residue dissolved in ethyl acetate and the solution washed with aqueous sodium carbonate and water. It is dried, evaporated, the residue triturated with isopropanol, filtered off and discarded. The filtrate is made strongly acidic with hydrogen chloride, the precipitate filtered off and triturated with 175 ml of boiling methanol, to yield the 1-[1-(4-amino-6,7-dimethoxy-2-quinazolinyl)-4-piperidinyl]-4,4-dimethyl-piperidin-2,6-dione monohydrochloride, melting at 279°-280° with decomposition.

WORKUP

后处理

  1. filtrationIt is filtered
  2. customthe filtrate evaporated
  3. dissolutionthe residue dissolved in ethyl acetate
  4. washthe solution washed with aqueous sodium carbonate and water
  5. customIt is dried
  6. customevaporated
  7. customthe residue triturated with isopropanol
  8. filtrationfiltered off
  9. filtrationthe precipitate filtered off
  10. customtriturated with 175 ml of boiling methanol