反应 #2206040
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US06812344B1
反应条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Scheme-III: A mixture of 1chloro-4-(2,5dioxopyrrolidin-1-yl)butane (11.0 g, 58.04 mmol), 1-[2-methoxyphenyl)piperizine hydrochloride (12.99 g, 56.85 minol), potassium carbonate (16.02 g, 116.09 mmol) and potassium iodide (0.577 g, 3.48 nmol) in N,N-dimethylformamide (45 ml) was stirred at 100° C. for 18 hours. N,N-dimethylformamide was evaporated at reduced pressure and the residue was taken up in water (100 ml) and extracted with chloroform (2×100 ml). The extracts were dried over Na2SO4 and concentrated under reduced pressure to give 1-[4(2-methoxyphenyl) piperizine 1-yl]4-(2,5-dioxopyrrolid-1-yl)butane as an oil which was purified by column chromatography over silica gel (230-400 mesh) using chloroform-methanol (98:2) as eluent; yield 18.00 g, (92%), oil. Hydrochloride salt was prepared by the method described above; mp 218-220° C. N,N-dimethylformamide was evaporated at reduced pressure extracted with chloroform (2×100 ml) The extracts were dried over Na2SO4 concentrated under reduced pressure
来源 ID: ord-f9fa64a2a07947a789833e97f5111b44