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1-(4-(2-fluoropyridin-3-yl)-5,6-dihydropyridin-1(2H)-yl)ethanone → 1-(4-(2-Fluoropyridin-3-yl)piperidin-1-yl)ethanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-(4-(2-fluoropyridin-3-yl)-5,6-dihydropyridin-1(2H)-yl)ethanone | HCID 59326965 | — |
| 触媒 | Palladium hydroxide | HCID 9942167 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-(4-(2-Fluoropyridin-3-yl)piperidin-1-yl)ethanone | HCID 58547834 | 196.2% |
反応手順
A 2 L Parr shaker bottle was charged with 1-(2-fluoro-5′,6′-dihydro-[3,4′-bipyridin]-1′(2′H)-yl)ethanone (see PREPARATION P14.1; 44.7 g, 0.203 mol), THF (600 mL), and palladium hydroxide on carbon, 20% wet type (22 g, 50 wt %). The bottle was purged three times with H2 and was shaken at room temperature under 50 psi of H2. At 1 hour, crude 1HNMR indicated full conversion (aliquot syringe filtered and concentrated). This reaction was filtered (along with another 44.7 g batch) through a CELITE® pad. The pad was washed with THF (2×250 mL). The filtrate was concentrated under vacuum to afford 88.5 g white solid (98% yield, >99% purity by LCMS, excellent purity by 1HNMR).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08497265B2 |
| 出典データセット | uspto-grants-2013_07 |
| ORD ID | ord-4f0d445e07ae4eb59c7ca6aae7eb23c0 |
| 出典メモ | uspto-grants-2013_07 |