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Sodium borohydride → Diethyl 2-(1-(tert-butoxycarbonyl)piperidin-4-yl)malonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 反応物 | Diethyl 2-(1-(tert-butoxycarbonyl)piperidin-4-ylidene)malonate | HCID 59605837 | — |
| 生成物 | Diethyl 2-(1-(tert-butoxycarbonyl)piperidin-4-yl)malonate | HCID 59605280 | 85% |
反応手順
To IMS (200 mL) at 0° C., NaBH4 (1.87 g, 0.047 mol) and a solution of 2-(1-(tert-butoxycarbonyl)piperidin-4-ylidene)malonic acid diethyl ester (17 g, 0.050 mol) in IMS (200 mL) were added. The resulting mixture was allowed to warm to ambient temperature and stirred for 1 h, then quenched with water and concentrated in vacuo. The resulting oil was then partitioned between EtOAc and water. The organic layer was separated and washed with brine, then dried (MgSO4) and concentrated in vacuo to afford the title compound as a yellow oil (14.6 g, 85%). LCMS (Method H): RT=3.90 min, [M+Na]+ 366.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08394796B2 |
| 出典データセット | uspto-grants-2013_03 |
| ORD ID | ord-a9865f61559241a29699f22d9698ecf0 |
| 出典メモ | uspto-grants-2013_03 |