反应 #1329303
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US05736550
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a solution of 1-(p-fluorobenzyl)-4-phthalimidopiperidine (3.0 g, 8.9 mmol) in ethanol (30 ml) was added hydrazine monohydrate (0.7 ml) and the mixture was heated under reflux for 3 hours. After allowed to cool, to the reaction mixture was added 5N hydrochloric acid (50 ml) and insolubles were filtered off. Then, the filtrate was washed with chloroform (30 ml×3). The aqueous layer was neutralized with potassium carbonate and then extracted with chloroform (50 ml×4). After drying over anhydrous magnesium sulfate, the solvent was distilled off to give 1.7 g of the title compound. Yield=94%. the mixture was heated under reflux for 3 hours to cool, to the reaction mixture were filtered off Then, the filtrate was washed with chloroform (30 ml×3) extracted with chloroform (50 ml×4) After drying over anhydrous magnesium sulfate the solvent was distilled off
来源 ID: ord-48123362fc86410da8f799ec9a7d74ad