29% |
With diphenyl ether-biphenyl eutectic; at 150℃; for 36.0h; |
To a solution of 6-chioro-3-amino-4,5-dimethyipyridazine (550 mg) in Dowtherm A (4 mL) was added ethyl 2-fluoro-3-oxo-butanoate (525 m) and the reaction was heated to 150 C for 18 hours. Additional ethyl 2-fluoro-3-oxo-butanoate (525 pL) was added and the reaction stirred for an additional 18 hours at 150 C. The reaction mixture was loaded directly onto a Teledyne ISCO Combi-Flash system (liquid loading with DCM, 120G column, 0-20% Hex/EtOAc, 6 min run; then 0-30% EtOAc/DCM, 10 min run) to afford the title compound (243 g; 29% yields NMR (400 MHz, CDCI3) d 2.62 (d, J = 0.9 Hz, 3H), 2.51 (d, J = 3.6 Hz, 3H), 2.48 (t, J = 0.9 |
29% |
With diphenyl ether-biphenyl eutectic; at 150℃; for 36.0h; |
To a solution of 6-chioro-3-amino-4,5-dimethyipyridazine (550 mg) in Dowtherm A (4 mL) was added ethyl 2-fluoro-3-oxo-butanoate (525 m) and the reaction was heated to 150 C for 18 hours. Additional ethyl 2-fluoro-3-oxo-butanoate (525 pL) was added and the reaction stirred for an additional 18 hours at 150 C. The reaction mixture was loaded directly onto a Teledyne ISCO Combi-Flash system (liquid loading with DCM, 120G column, 0-20% Hex/EtOAc, 6 min run; then 0-30% EtOAc/DCM, 10 min run) to afford the title compound (243 g; 29% yields NMR (400 MHz, CDCI3) d 2.62 (d, J = 0.9 Hz, 3H), 2.51 (d, J = 3.6 Hz, 3H), 2.48 (t, J = 0.9 |
29% |
at 150℃; for 36.0h; |
To a solution of 6-chioro-3-amino-4,5-dimethyipyridazine (550 mg) in Dowtherm A (4 mL) was added ethyl 2-fluoro-3-oxo-butanoate (525 m) and the reaction was heated to 150 C for 18 hours. Additional ethyl 2-fluoro-3-oxo-butanoate (525 pL) was added and the reaction stirred for an additional 18 hours at 150 C. The reaction mixture was loaded directly onto a Teledyne ISCO Combi-Flash system (liquid loading with DCM, 120G column, 0-20% Hex/EtOAc, 6 min run; then 0-30% EtOAc/DCM, 10 min run) to afford the title compound (243 g; 29% yields NMR (400 MHz, CDCI3) d 2.62 (d, J = 0.9 Hz, 3H), 2.51 (d, J = 3.6 Hz, 3H), 2.48 (t, J = 0.9 |