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8-[2-(6,6-Dimethyl-bicyclo[3.1.1]hept-2-yl)-ethyl]-3-(3-methylamino-propyl)-1-phenyl-1,3,8-triaza-spiro[4.5]decan-4-one → 4-{[(3-{8-[2-(6,6-Dimethyl-bicyclo(3.1.1]hept-2-yl)-ethyl]-4-oxo-1-phenyl-1,3,8-triaza-spiro[4.5]dec-3-yl} propyl)-methyl-amino]-methyl}-4-hydroxy-piperidine-1-carboxylic Acid Tert-Butyl Ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 8-[2-(6,6-Dimethyl-bicyclo[3.1.1]hept-2-yl)-ethyl]-3-(3-methylamino-propyl)-1-phenyl-1,3,8-triaza-spiro[4.5]decan-4-one | HCID 11236337 | — |
| 反応物 | tert-Butyl 1-oxa-6-azaspiro(2.5)octane-6-carboxylate | HCID 22135564 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4-{[(3-{8-[2-(6,6-Dimethyl-bicyclo(3.1.1]hept-2-yl)-ethyl]-4-oxo-1-phenyl-1,3,8-triaza-spiro[4.5]dec-3-yl} propyl)-methyl-amino]-methyl}-4-hydroxy-piperidine-1-carboxylic Acid Tert-Butyl Ester | HCID 58906460 | 89.8% |
反応手順
2.6 g (5.74 mmol) of compound (24) was placed in a flask and diluted with 20 ml ethanol. To this solution was added 1.88 g (8.81 mmol) of the epoxide (32) and the mixture was heated to reflux until TLC showed complete conversion. For work-up the solvent was evaporated and the residue was taken up with ethyl acetate. After washing with aqueous potassium carbonate solution drying over sodium sulphate and concentration in vacuo the raw material was purified via flash column chromatography yielding a light yellow viscous oil (3.51 g, 5.15 mmol, 89.8% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07241770B2 |
| 出典データセット | uspto-grants-2007_07 |
| ORD ID | ord-67eb260948ba40f785b3601cea271b8b |
| 出典メモ | uspto-grants-2007_07 |