反应详情

Diethyl azodicarboxylate (100 μl; 0.63 mmol) was added dropwise to a solution of 7-hydroxy-4-(2-methoxyethylsulphanyl)quinazoline (100 mg, 0.42 mmol), (prepared as described for the starting material in Example 11), 3-(1,1-dioxothiomorpholino)-1-propanol (99 mg, 0.51 mmol) and triphenylphosphine (167 mg, 0.63 mmol) in methylene chloride (6 ml). After stiring for 4 hours, triphenylphosphine (167 mg, 0.63 mmol) and diethyl azodicarboxylate (100 μl, 0.63 mmol) were added and stirring was continued for 1 hour. The volatiles were removed by evaporation and the residue was purified by column chromatography eluting with ethyl acetate/methanol (100/0 followed by 92/8). After removal of the solvent by evaporation, the residue was triturated with ether and the solid was collected by filtration and dried under vacuum to give 7-(3-(1,1-dioxothiomorpholino)propoxy)4-(2-methoxyethylsulphanyl)quinazoline (72 mg, 41%).

1. custom(prepared
2. waitwas continued for 1 hour
3. customThe volatiles were removed by evaporation
4. customthe residue was purified by column chromatography
5. washeluting with ethyl acetate/methanol (100/0 followed by 92/8)
6. customAfter removal of the solvent
7. customby evaporation
8. customthe residue was triturated with ether
9. filtrationthe solid was collected by filtration
10. customdried under vacuum