反应详情

温度

60 °C

A mixture of 2-chloro-5-[(tetrahydro-2H-pyran-2-yloxy)methyl]-1,3-thiazole (10.4 g), 10% palladium carbon (containing 50% water, 2.0 g), potassium carbonate (6.2 g) and methanol (10 mL) was stirred under hydrogen atmosphere (5 atm) at 60° C. for 10 hr. The insoluble material was filtered off, and the filtrate was concentrated. Water was added to the residue, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with saturated brine, dried (MgSO4) and concentrated. The obtained residue was subjected to silica gel column chromatography, and the title compound (6.97 g, yield 79%) was obtained as a colorless oil from a fraction eluted with ethyl acetate-hexane (1:2, volume ratio).

1. filtrationThe insoluble material was filtered off
2. concentrationthe filtrate was concentrated
3. additionWater was added to the residue
4. extractionthe mixture was extracted with ethyl acetate
5. washThe ethyl acetate layer was washed with saturated brine
6. dry with materialdried (MgSO4)
7. concentrationconcentrated