関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | N-(1-benzylpiperidin-4-yl)-2,2,2-trifluoroacetamide | HCID 1531300 | — |
| 反応物 | Ammonium formate | HCID 2723923 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2,2,2-trifluoro-N-(piperidin-4-yl)acetamide | HCID 10774253 | — |
反応手順
A 500 mL, three-necked round-bottomed flask under nitrogen was charged with 4 g of 10% Palladium on Carbon, and 100 mL of methanol. The suspension was cooled to 5° C. and 10 g of ammonium formate was added in one batch (evolution of gas was observed). A solution of 10 g (35 mmol) of the 4-trifluoroacetamido-1-benzylpiperidine in 100 mL of methanol was then added dropwise gradually. The resulting reaction mixture was refluxed for 2.5 hr. and then at room temperature overnight. The catalyst was filtered off through Celite under a blanket of nitrogen and washed with ethanol. The filtrate was concentrated under reduced pressure to give 6.9 g (quantitative yield) of a light yellow solid of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06506749B2 |
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| 出典データセット | uspto-grants-2003_01 |
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| ORD ID | ord-dfd2ecebe6804fa5b1cb67b841bed5d8 |
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| 出典メモ | uspto-grants-2003_01 |
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