Ethyl Acetate → 1-(2,4-Difluorophenyl)-6-fluoro-1,4-dihydro7-(5((5-methyl-2-oxo-1,3-dioxolen-4-yl)methyl)-2,5diazabicyclo(2.2.1)-hept-2-yl)-4-oxoquinoline-3-carboxylic acid

참여 물질

반응 단계

To 188 mg (0.434 m Mol) of 7-(2,5-diazabicyclo(2.2.1)hept-2-yl)-6-fluoro-1-(2,4-difluorophenyl)-1,4-di-hydro-4-oxoquinoline-3-carboxylic acid monohydrate (Example 11) was suspended in 20 ml dry DMF was added 96 mg (0.95 m Mol) anhydrous calcium bicarbonate and 92 mg (0.48 m Mol) 4-bromomethyl-5-methyl-1,3-dioxolen-2-one. The resultant suspension was stirred at room temperature for 10 hrs. Then the suspension was treated with 150 ml of ethyl acetate and 50 ml of water. The organic phase was separated and washed with 5×30 ml water, dried over sodium sulfate, filtered the volatiles were removed at room temperature under reduced pressure. Recrystallization from ethyl acetate gave 63 mg (27.5%) of the desired material.

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