2-甲氧基-2H-吡喃-5-one

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 6-methoxy-2H-pyran-3(6H)-one 12.8 (0.1 mole) in 40 ml CH2Cl2 at 0° C. was added 16.0 g (0.1 mole) of bromine in 10 ml of CH2Cl2. Then 14 ml of triethylamine was added dropwise at 0° C. and the reaction was allowed to warm to room temperature and stir for two hours. The reaction was then diluted with 200 ml of toluene. After filtration, the organic solution was then washed with 5% NaHCO3 and brine, dried with Na2SO4, filtered and concentrated to yield the crude product as light brown solid Recrystallisation from ethyl acetate afforded the title compound (17 g, 82%) as a white crystalline solid. m.p. 74-75° C. After filtration the organic solution was then washed with 5% NaHCO3 and brine dried with Na2SO4 filtered concentrated to yield the crude product as light brown solid Recrystallisation from ethyl acetate

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 6-methoxy-2H-pyran-3(6H)-one 12.8 (0.1 mole) in 40 ml CH2Cl2 at 0° C. was added 16.0 g (0.1 mole) of bromine in 10 ml of CH2Cl2. Then 14 ml of triethylamine was added dropwise at 0° C. and the reaction was allowed to warm to room temperature and stir for two hours. The reaction was then diluted with 200 ml of toluene. After filtration, the organic solution was then washed with 5% NaHCO3 and brine, dried with Na2SO4, filtered and concentrated to yield the crude product as light brown solid. Recrystallisation from ethyl acetate afforded the title compound (17 g 82%) as a white crystalline solid. After filtration the organic solution was then washed with 5% NaHCO3 and brine dried with Na2SO4 filtered concentrated to yield the crude product as light brown solid Recrystallisation from ethyl acetate

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 6-methoxy-2H-pyran-3(6H)-one 12.8 (0.1 mole) in 40 ml CH2Cl2 at 0° C. was added 16.0 g (0.1 mole) of bromine in 10 ml of CH2Cl2. Then 14 ml of triethylamine was added dropwise at 0° C. and the reaction was allowed to warm to room temperature and stir for two hours. The reaction was then diluted with 200 ml of toluene. After filtration, the organic solution was then washed with 5% NaHCO3 and brine, dried with Na2SO4, filtered and concentrated to yield the crude product as light brown solid. Recrystallisation from ethyl acetate afforded the title compound (17 g, 82%) as a white crystalline solid. m.p. 74-75° C. After filtration the organic solution was then washed with 5% NaHCO3 and brine dried with Na2SO4 filtered concentrated to yield the crude product as light brown solid Recrystallisation from ethyl acetate