関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-(1-Pyrrolidinyl)piperidine | HCID 78703 | — |
| 反応物 | [4-(4-Nitrophenoxy)pyridin-2-yl]carbamic acid phenyl ester | HCID 57677544 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 86602163 | HCID 86602163 | — |
反応手順
[4-(4-Nitrophenoxy)pyridin-2-yl]carbamic acid phenyl ester (100 mg) was dissolved in tetrahydrofuran (2 ml) under a nitrogen atmosphere, and then 4-(pyrrolidin-1-yl)piperidine (148 mg) was added thereto, followed by stirring for 50 min. The reaction mixture was partitioned between ethyl acetate and a saturated aqueous solution of ammonium chloride. The organic layer was washed with a saturated aqueous solution of ammonium chloride, water and brine in this order, and dried over anhydrous sodium sulfate. The solvent was evaporated under a reduced pressure to give a residue, which was then purified by silica gel column chromatography (Fuji Silysia NH, eluent; hexane:ethyl acetate=1:2 to 1:8). The solvent was evaporated under a reduced pressure to give a residue, which was then dried in vacuum to provide 4-(pyrrolidin-1-yl)piperidine-1-carboxylic acid [4-(4-nitrophenoxy)pyridin-2-yl]amide as a crude product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07531532B2 |
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| 出典データセット | uspto-grants-2009_05 |
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| ORD ID | ord-d5e3f660a42a46ca8ffcc9ed43bd1958 |
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| 出典メモ | uspto-grants-2009_05 |
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