反应详情

温度

0 °C

A 100 mL flask was charged with 6-chloro-4-methylpyridazin-3-amine (700 mg, 4.88 mmol) and pyridine (20 mL) then ethyl chloroformate (0.421 mL, 4.39 mmol) was added portionwise. The reaction mixture was stirred for 1 h at 0° C. The reaction mixture was then concentrated and partitioned between ammonium chloride and DCM. The aqueous layer was extracted with DCM (2×). The organic layers were combined and washed with brine (1×), eluted through a phase separator and concentrated to afford ethyl (6-chloro-4-methylpyridazin-3-yl)carbamate (549 mg, 49.6% yield).

1. concentrationThe reaction mixture was then concentrated
2. custompartitioned between ammonium chloride and DCM
3. extractionThe aqueous layer was extracted with DCM (2×)
4. washwashed with brine (1×)
5. washeluted through a phase separator
6. concentrationconcentrated