反应详情

A stirred solution of 4-methyl-5-pyridin-4-yl-thiazol-2-ylamine (prepared according to the method described in European patent specification EP 117082 A2) (0.068 g, 3.56 mmol) in DMF (5 ml) is treated with ethyl isocyanatoacetate (0.043 ml, 3.916 mmol) and the solution is stirred overnight. The solvent is removed in vacuo and the crude product is partitioned between ethyl acetate (50 ml) and water (50 ml). The layers are separated and the aqueous portion is extracted with ethyl acetate (2×50 ml). The combined organic portions are washed with water, dried (MgSO4), filtered and concentrated in vacuo to yield an oil. Trituration with ethyl acetate yields the titled compound.

1. customThe solvent is removed in vacuo
2. customthe crude product is partitioned between ethyl acetate (50 ml) and water (50 ml)
3. customThe layers are separated
4. extractionthe aqueous portion is extracted with ethyl acetate (2×50 ml)
5. washThe combined organic portions are washed with water
6. dry with materialdried (MgSO4)
7. filtrationfiltered
8. concentrationconcentrated in vacuo
9. customto yield an oil