반응 #51058

반응 방정식

hydrogen chloride

7-(2-acetoxy-3-morpholinopropoxy)-4-(3-chlorobenzofuran-7-ylamino)-6-methoxyquinazoline dihydrochloride

ammonia

Diethyl ether

→

title compound

수율 157.7%

4-(3-chlorobenzofuran-7-ylamino)-7-(2-hydroxy-3-morpholinopropoxy)-6-methoxyquinazoline dihydrochloride salt

수율 157.7%

용매

isopropanol

methylene chloride

반응 조건

후처리

1. 1
   기타The solvent was evaporated
2. 2
   workup.DISSOLUTIONthe residue was dissolved in methylene chloride (3 ml)
3. 3
   세척9470-0100) and eluted with a 19:1 mixture of methylene chloride and methanol
4. 4
   기타The material so obtained
5. 5
   여과the resultant precipitate was collected by filtration
6. 6
   세척washed with diethyl ether
7. 7
   기타dried under vacuum

실험 절차

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.

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