反应 #2021049
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07851473B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a solution of N-1,2-benzisoxazol-3-ylpiperazine-1-carboxamide trifluoroacetate (200 mg, 0.555 mmol) and triethylamine (0.309 ml, 2.22 mmol) in tetrahydrofuran (4 ml) was added 3-fluorobenzyl chloroformate (157 mg, 0.833 mmol) under ice-cooling, and the mixture was stirred at room temperature for 1 hour. The reaction mixture was poured to water and extracted with ethyl acetate. The extract was washed with water, and the solvent was distilled off under reduced pressure. The residue was recrystallized from a mixed solvent of hexane and ethyl acetate to give 132 mg (59.7%) of the desired product as a solid. cooling extracted with ethyl acetate The extract was washed with water the solvent was distilled off under reduced pressure The residue was recrystallized from a mixed solvent of hexane and ethyl acetate
来源 ID: ord-ea720f9ed97c41f2ba3322eda02efd01