反应详情

A suspension of methyl 3-chloro-7-(2,2-dimethylpropionylamino)-10H-9-oxa-1,2-diazaphenanthrene-8-carboxylate (Intermediate 8, 1.01 g), ammonium formate (0.848 g) and 10% palladium on carbon (0.150 g) in ethanol (60 mL) was stirred and heated at reflux under nitrogen for one hour. After cooling, the suspension was filtered and the filtrate was evaporated. The residue was dissolved in ethyl acetate and washed with water (with warming to dissolve all of the solid), dried (Na2SO4) and filtered. The filtrate was evaporated in vacuo and the residue was triturated with ether. The solid was collected by filtration and purified by chromatography on silica, eluting with ethyl acetate to give methyl 7-(2,2-dimethylpropionylamino)-10H-9-oxa-1,2-diazaphenanthrene-8-carboxylate (0.705 g) as a white solid.

1. temperatureheated
2. temperatureat reflux under nitrogen for one hour
3. temperatureAfter cooling
4. filtrationthe suspension was filtered
5. customthe filtrate was evaporated
6. dissolutionThe residue was dissolved in ethyl acetate
7. washwashed with water (
8. temperaturewith warming
9. dissolutionto dissolve all of the solid),
10. dry with materialdried (Na2SO4)
11. filtrationfiltered
12. customThe filtrate was evaporated in vacuo
13. customthe residue was triturated with ether
14. filtrationThe solid was collected by filtration
15. custompurified by chromatography on silica
16. washeluting with ethyl acetate