反应详情

A solution of tert-butyl 2-(6-(dimethylcarbamoyl)-2-morpholino-4-oxo-4H-chromen-8-yl)-1H-pyrrole-1-carboxylate (0.6 g, 1.28 mmol) in MeOH (10 mL) was hydrogenated over 5% Rh/Al2O3 (NanoThales CatCart cartridge, product ID THS 02118) with the H-Cube (Continuous flow hydrogenation apparatus HC-2.5S from THALES Nanotechnology Inc. Budapest H-1031; Zahony u.7.; Hungaria) at 10 bars, 50° C. and a flow rate of 1 mL/min. for 3.5 h with continuous recycling. The cartridge was replaced by a 10% Pd/c cartridge and hydrogenation was pursued for 6 h at 60 bars and 60° C. The mixture was evaporated to dryness to give a solid which was triturated in diethyl ether, filtered and dried under vacuum at 50° C. to afford pure tert-butyl 2-(6-(dimethylcarbamoyl)-2-morpholino-4-oxo-4H-chromen-8-yl)pyrrolidine-1-carboxylate (0.30 g, 50%) as a white solid. The crude product was used as such for the next step. Mass Spectrum: m/z [M+H]+=472.

1. waitwas pursued for 6 h at 60 bars and 60° C
2. customThe mixture was evaporated to dryness
3. customto give a solid which
4. customwas triturated in diethyl ether
5. filtrationfiltered
6. customdried under vacuum at 50° C.