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2-(Pyridin-3-yl)ethan-1-amine → {2-[(9R)-9-(pyridin-2-yl)-6-oxaspiro[4.5]decan-9-yl]ethyl}[2-(pyridin-3-yl)ethyl]amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-(Pyridin-3-yl)ethan-1-amine | HCID 854051 | — |
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 反応物 | 2-[(9R)-9-pyridin-2-yl-6-oxaspiro[4.5]decan-9-yl]acetaldehyde | HCID 86671427 | — |
| 触媒 | Methanol | HCID 887 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | {2-[(9R)-9-(pyridin-2-yl)-6-oxaspiro[4.5]decan-9-yl]ethyl}[2-(pyridin-3-yl)ethyl]amine | HCID 68314495 | — |
反応手順
To a solution of 2-[(9R)-9-(pyridin-2-yl)-6-oxaspiro[4.5]decan-9-yl]acetaldehyde (50 mg, 0.19 mmole), 5 mL DCM and NA2SO4 (134 mg, 0.95 mmole) was added 2-(pyridin-3-yl)ethan-1-amine (31 mg, 0.25 mmole) and the reaction was stirred overnight. NaBH4 (9.5 mg, 0.25 mmole) added, stir 10 minutes, 2 drops MeOH added, stir 1 h, quenched with water, organics separated off and evaporated. The residue was passed through a Gilson reverse phase HPLC to give {2-[(9R)-9-(pyridin-2-yl)-6-oxaspiro[4.5]decan-9-yl]ethyl}[2-(pyridin-3-yl)ethyl]amine, 65.3 mg (71%). LCMS m/z 367.1 (M+1) observed.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08835488B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-7e83c6038e084f6d92a93b7c8b081ab8 |
| 出典メモ | uspto-grants-2014_09 |