反应详情

A solution of aminopyridine (3) (0.94 g, 5.49 mmol), ethyl chloroacetylcarbamate (1.09 g, 6.58 mmol) and 2,6-lutidine (0.76 mL, 6.58 mmol) in 1,3-dimethyl-2-imidazolidinone (6 mL) was warmed under nitrogen at 110° C. for 4.5 hours. The mixture was diluted with EtOAc and washed with water (6 times), then adsorbed onto silica by removal of solvent in vacuo. The product was chromatographed on silica. Elution with EtOAc gave foreruns, while MeOH/EtOAc (2:23) eluted product (79 mg, 5%) as a solid, mp 248-252° C. (decomposed).

1. washwashed with water (6 times)
2. customadsorbed onto silica by removal of solvent in vacuo
3. customThe product was chromatographed on silica
4. washElution with EtOAc
5. customgave foreruns
6. washwhile MeOH/EtOAc (2:23) eluted product (79 mg, 5%) as a solid, mp 248-252° C. (decomposed)