反応 #1701155
関連文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08183380B2
反応条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a solution of [1-(2-hydroxy-ethyl)-piperidin-4-yl]-carbamic acid tert-butyl ester (CAS m 558443-53-1) (5.71 g, 23 mmol) in tetrahydrofuran (100 ml) at 23° C. was added in portions lithium aluminum hydride (2.66 g, 70 mmol) and the mixture was stirred at 70° C. for 18 h. Then the reaction was cooled to 0° C., water (2.66 ml) was added very slowly, then NaOH 15% (7.98 ml) and water (2.66 ml). The mixture was stirred at 23° C. for 1.5 h, the precipitate was filtered off, washed with tetrahydrofuran and the organic layer was evaporated totally to give the title compound as a white solid (3.7 g, 100%), MS (ISP) m/e=159.3 [(M+H)+]. Then the reaction was cooled to 0° C. The mixture was stirred at 23° C. for 1.5 h the precipitate was filtered off washed with tetrahydrofuran the organic layer was evaporated totally
ソース ID: ord-f706bef6a8d14cf3ab32a18d2dfaa3f2