HRID22780

反应详情

EQUATION

反应方程式

HRID 22780 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 7-(2-acetoxy-3-morpholinopropoxy)-4-(3-chlorobenzofuran-7-ylamino)-6-methoxyquinazoline dihydrochloride (0.15 g) and a saturated methanolic ammonia solution (3 ml) was stirred at ambient temperature overnight. The solvent was evaporated and the residue was dissolved in methylene chloride (3 ml) and adsorbed to the top of a pre-packed silica column (NH2-silica; Isolute sorbent from International Sorbent Technology Ltd, ref. no. 9470-0100) and eluted with a 19:1 mixture of methylene chloride and methanol. The material so obtained was dissolved in methylene chloride (3 ml) and a 6M solution of hydrogen chloride in isopropanol (0.3 ml) was added. Diethyl ether (10 ml) was added and the resultant precipitate was collected by filtration, washed with diethyl ether and dried under vacuum. There was thus obtained the title compound (0.11 g); Mass Spectrum: M+H+ 486.

WORKUP

后处理

  1. customThe solvent was evaporated
  2. dissolutionthe residue was dissolved in methylene chloride (3 ml)
  3. wash9470-0100) and eluted with a 19:1 mixture of methylene chloride and methanol
  4. customThe material so obtained
  5. filtrationthe resultant precipitate was collected by filtration
  6. washwashed with diethyl ether
  7. customdried under vacuum