関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyrrolidine | HCID 31268 | — |
| 反応物 | Dimethylformamide dimethyl acetal | HCID 78373 | — |
| 反応物 | 2-Methoxy-4-methyl-5-nitropyridine | HCID 243169 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 5-methoxy-1H-pyrrolo(2,3-c)pyridine | HCID 641092 | — |
反応手順
10.76 g of N,N-dimethylformamide dimethyl acetal and 2.45 ml of pyrrolidine are added, in succession, to a solution of 5 g of the product obtained in Step 1 in 60 ml of dimethylformamide. The mixture obtained is first heated at 100° C. for 8 hours and then at 150° C. for 1 hour. Concentration is carried out under a vacuum of 10−1 mbar and the residue is taken up in 150 ml of tetrahydrofuran. The solution obtained is hydrogenated under a pressure of 10 bars for 4 hours in the presence of 10% Pd/C. After filtration and concentration, the residue is chromatographed over silica (eluant CH2Cl2/EtOH: 95/5) to yield the expected product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06566364B2 |
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| 出典データセット | uspto-grants-2003_05 |
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| ORD ID | ord-a3061b7900ab4dd4bb7e76ad2c4cb10f |
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| 出典メモ | uspto-grants-2003_05 |
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