反应详情

To a stirred mixture of 3-amino-4-methoxypyridine (2.01 g, 16.2 mmol) and NaHCO3 (4.08 g, 48.6 mmol) in CHCl3 and water (1:1, 50 mL) at 4° C. was added thiophosgene (1.5 mL, 19.6 mmol) dropwise. After completion of the addition, the ice bath was removed. The mixture was stirred for 4 hours, the organic layer was separated, and the aqueous layer was extracted with CH2Cl2. The combined organic phases were washed with water, dried over Na2SO4, filtered, and concentrated to give the title compound as brown solid.

1. additionAfter completion of the addition
2. customthe ice bath was removed
3. customthe organic layer was separated
4. extractionthe aqueous layer was extracted with CH2Cl2
5. washThe combined organic phases were washed with water
6. dry with materialdried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated