反应详情

温度

110 °C

A mixture of diethyl N-{p-[N-((6RS)-2-methyl-4-oxo-3-pivaloyloxymethyl-3,4,7,8-tetrahydro-6H-cyclopenta[g]quinazolin-6-yl)amino]benzoyl}-L-glutamate (13.5 g), propargyl bromide (32 g), calcium carbonate (10.7 g) and DMA (250 ml) was stirred and heated to 110° C. for 5 hours. The mixture was evaporated and the residue was partitioned between ethyl acetate and water. The organic phase was washed with water, dried (MgSO4) and evaporated. The residue was purified by column chromatography using increasingly polar mixtures of hexane and ethyl acetate as eluant. There was thus obtained diethyl -{p-[N-((6RS)-2-methyl-4-oxo-3-pivaloyloxymethyl-3,4,7,8-tetrahydro-6H-cyclopenta[g]quinazolin-6-yl)-N-(prop-2-ynyl)--amino]benzoyl }-L-glutamate as a foam (9 g).

1. customThe mixture was evaporated
2. customthe residue was partitioned between ethyl acetate and water
3. washThe organic phase was washed with water
4. dry with materialdried (MgSO4)
5. customevaporated
6. customThe residue was purified by column chromatography
7. temperatureusing increasingly polar mixtures of hexane and ethyl acetate as eluant