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HRID 609597作成日:2026年10月26日

N-[(1-benzyl-4-piperidyl)methyl] 3,4-dihydro-2H-[1,3]oxazino[3,2-a]indole-10-carboxamide oxalate salt → N-(4-Piperidylmethyl) 3,4-dihydro-2H-[1,3]oxazino[3,2-a]indole-10-carboxamide

https://huagongshe.com/reaction/609597

反応式

関与物質

役割名称HCID仕込み量
反応物N-[(1-benzyl-4-piperidyl)methyl] 3,4-dihydro-2H-[1,3]oxazino[3,2-a]indole-10-carboxamide oxalate saltHCID 19599416—
触媒PalladiumHCID 23938—
溶媒Acetic AcidHCID 176—
溶媒EthanolHCID 702—
生成物N-(4-Piperidylmethyl) 3,4-dihydro-2H-[1,3]oxazino[3,2-a]indole-10-carboxamideHCID 9839803105.4%

反応手順

A stirred suspension of N-[(1-benzyl-4-piperidyl)methyl] 3,4-dihydro-2H-[1,3]oxazino[3,2-a]indole-10-carboxamide oxalate salt (E20, 2.25 g, 0.0046 mole) in ethanol (100 ml) and glacial acetic acid (4 ml) was hydrogenated over 10% Pd-C (0.8 g) at atmospheric pressure and 45° C. for 18 h. The mixture was filtered and the filtrate concentrated in vacuo. The majority of the product was in the solid which had been filtered off. This material was shaken with concentrated potassium carbonate solution (50 ml) and chloroform (50 ml) together with the residue from the filtrate. The mixture was filtered, the chloroform layer separated and dried (Na2SO4), then concentrated in vacuo to afford the title compound as a white solid (1.52 g, 100%). This was recrystallised from chlorofornm/60-80 petrol mp 139-141° C.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05998409
出典データセットuspto-grants-1999_12
ORD IDord-ed20c27d31994e61b67e037e60ae3473
出典メモuspto-grants-1999_12