反应 #1500673
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US06838581B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a THF solution of (R)-3-phenyl-3-hydroxypropanenitrile was slowly added borane dimethyl sulfide complex at room temperature. Methyl sulfide was then distilled from the reaction vessel and the resulting THF solution refluxed for 2.5 h. After cooling to room temperature methanolic HCl was added to the reaction mixture. Methanol and methyl borate were removed by distillation and the reaction mixture neutralized with sodium hydroxide (5N). Extraction of the mixture with dichloromethane followed by concentration provided the crystalline (R)-3-phenyl-3-hydroxypropylamine. at room temperature Methyl sulfide was then distilled from the reaction vessel the resulting THF solution refluxed for 2.5 h was added to the reaction mixture Methanol and methyl borate were removed by distillation Extraction of the mixture with dichloromethane followed by concentration
来源 ID: ord-01e61fc24ffa4f8b9dad05e8e43cf03c