反应详情

A solution of ethyl 5-(aminothioxomethyl)tetrahydro-2H-1,2-oxazine-2-carboxylate (i.e. the product of Step I) (0.19 g, 0.87 mmol) and 2-bromo-1-(4,5-dihydro-5-(2,6-difluorophenyl)-3-isoxazolyl)ethanone (the product of Example 1, Step C) (0.264 g, 0.87 mmol) in methanol (2 mL) was heated at 50° C. for 1 h. Methanol was removed under reduced pressure and the resulting material was partitioned between sodium acetate (10%, 5 mL) and diethyl ether (5 mL). The layers were separated and the aqueous phase was extracted with diethyl ether (2×). The organic fractions were concentrated under reduced pressure to provide the title compound as a pale-tan oil (0.383 g).

1. customMethanol was removed under reduced pressure
2. customthe resulting material was partitioned between sodium acetate (10%, 5 mL) and diethyl ether (5 mL)
3. customThe layers were separated
4. extractionthe aqueous phase was extracted with diethyl ether (2×)
5. concentrationThe organic fractions were concentrated under reduced pressure