反应详情

温度

-78 °C

A 1.55M solution of butyllithium (10 ml, 15.5 mmol) in hexane was added by syringe to a stirred solution of (2R)-2,5-dihydro-3,6-dimethoxy-2-isopropylpyrazine (2.85 g, 15.5 mmol) in THF (50 ml) at -78° C. and the solution stirred for 1 hour at -78° C. A solution of 4- chloromethyl-3,5-dimethylisoxazole (2.34 g, 16 mmol) in THF (10 ml) was added gradually and the stirring continued overnight. The solvent was removed under reduced pressure, the residue dissolved in ethyl acetate (50 ml) and extracted with phosphate buffer (pH 7). The water phase was extracted twice with ethyl acetate (2×20 ml). The organic layer was dried (MgSO4), solvent evaporated under reduced pressure and the residue purified by flash chromatography (diethyl ether/hexane 4/1, silica gel).

1. customthe stirring continued overnight
2. customThe solvent was removed under reduced pressure
3. dissolutionthe residue dissolved in ethyl acetate (50 ml)
4. extractionextracted with phosphate buffer (pH 7)
5. extractionThe water phase was extracted twice with ethyl acetate (2×20 ml)
6. dry with materialThe organic layer was dried (MgSO4), solvent
7. customevaporated under reduced pressure
8. customthe residue purified by flash chromatography (diethyl ether/hexane 4/1, silica gel)