反应 #1489199
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US09156798B2
反应条件: temp:10.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a suspension of lithium aluminum hydride (2.8 equiv.) in dry THF (1.7 M) was added a solution of crude methyl 3-amino-2,2-dimethylcyclobutanecarboxylate (1.0 equiv.) in dry THF (0.7 M) at 0° C. Then the mixture was stirred under vigorously at 10° C. for 0.5 h, and then heated to 35-40° C. for 12 h. The reaction was quenched by addition of water, aqueous sodium hydroxide solution (3N) slowly at 0° C., and water. The mixture was stirred at 10° C. for 20 min, filtered through celite, and washed with ethyl acetate. The organic phase was dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated in vacuo to give the crude title compound (3-amino-2,2-dimethylcyclobutyl)methanol as a racemic mixture (89.7% yield). heated to 35-40° C. for 12 h The reaction was quenched by addition of water, aqueous sodium hydroxide solution (3N) slowly at 0° C. The mixture was stirred at 10° C. for 20 min filtered through celite washed with ethyl acetate The organic phase was dried over anhydrous sodium sulfate filtered The filtrate was concentrated in vacuo
来源 ID: ord-cf1e7cf9d87b4cec9d2bc58f45619772