反应 #1329312
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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 THF (200 ml) was added a small amount of lithium aluminum hydride, the solvent was dried, lithium aluminum hydride (2.0 g, 53 mmol) was suspended and the mixture was stirred at room temperature. Crystals of 4-(p-fluorobenzyl)-3-nitromethylidenemorpholine (6.58 g, 26.1 mmol) was added gradually and the mixture was stirred at room temperature. A further amount of lithium aluminum hydride (1.3 g, 34 mmol) was added and the mixture was stirred for one hour. Water (3.3 ml), 40% aqueous NaOH (3.3 ml) and water (10 ml) were added in turn and then potassium carbonate (40 g) was added followed by stirring. The reaction mixture was filtered and distilled off. The residue was dissolved in chloroform, dried over potassium carbonate and then the chloroform was distilled off to give 5.44 g of 3-aminomethy-4-(p-fluorobenzyl)morpholine as an oily substance. Yield=93%. the solvent was dried the mixture was stirred at room temperature the mixture was stirred for one hour by stirring The reaction mixture was filtered distilled off The residue was dissolved in chloroform dried over potassium carbonate the chloroform was distilled off
来源 ID: ord-edfcefce95b94145b868512cf996e758