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0 °C

To a 100 mL flask was added 4-methyl-6-(methyloxy)-3-pyridinamine (850 mg, 6.15 mmol), pyridine (10 mL) and then ethyl chloroformate (0.650 mL, 6.77 mmol) 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, and the aqueous layer was extracted with DCM (2×). The combined organics layers were washed with brine (1×), eluted through a phase separator then concentrated to afford ethyl [4-methyl-6-(methyloxy)-3-pyridinyl]carbamate (1.223 g, 90% 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. washThe combined organics layers were washed with brine (1×)
5. washeluted through a phase separator
6. concentrationthen concentrated