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Trifluoroacetic acid → Benzyl 4-(2-chloro-pyridin-3-yl-amino)-piperidine-1-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trifluoroacetic acid | HCID 6422 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2-Chloro-3-pyridylamine | HCID 80528 | — |
| 反応物 | Benzyl 4-oxopiperidine-1-carboxylate | HCID 643496 | — |
| 反応物 | Sodium triacetoxyborohydride | HCID 5049666 | — |
| 溶媒 | Isopropyl Acetate | HCID 7915 | — |
| 生成物 | Benzyl 4-(2-chloro-pyridin-3-yl-amino)-piperidine-1-carboxylate | HCID 46853853 | — |
反応手順
560 mL (7.25 mol) TFA were added dropwise at approx. 15° C. to 930 g (3.99 mol) N-benzyloxy carbonyl-4-piperidone and 466 g (3.63 mol) 2-chloro-3-aminopyridine in 9.5 L isopropyl acetate. 922 g (4.35 mol) sodium triacetoxyborohydride were added batchwise. The mixture was stirred until the reaction was complete. At RT the reaction mixture was combined with 860 mL sodium hydroxide solution (2 mol/L). The organic phase was separated off, washed with 5 L water and evaporated down.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08829006B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-a06270afeed240be97e9dcae3d8058fa |
| 出典メモ | uspto-grants-2014_09 |