関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Methyl 2-Chloro-6-methylisonicotinate | HCID 2759833 | — |
| 触媒 | Zinc cyanide (Zn(CN)2) | HCID 11186 | — |
| 生成物 | Methyl 2-cyano-6-methylisonicotinate | HCID 58802283 | — |
反応手順
Under N2, methyl 2-chloro-6-methylisonicotinate (CAS 3998-90-1) (1.000 g, 5.39 mmol, Eq: 1.00), zinc cyanide (759 mg, 6.47 mmol, Eq: 1.2) and Tetrakis-triphenylphosphin-palladium (623 mg, 539 μmol, Eq: 0.1) were mixed in DMF (17 ml). The RM was stirred under microwave at 160° C. for 30 minutes. Control with TLC: the reaction was finished. The RM was partitioned between EtOAc and water; extracted; the organic phase was dried over MgSO4; filtered; concentrated in vacuo. The crude material was purified by flash chromatography (silica gel, 100 g, 5% to 30% EtOAc in heptane). Purple solid. MS (ISP): 177.2 ([M+H]+)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09029370B2 |
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| 出典データセット | uspto-grants-2015_05 |
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| ORD ID | ord-8aad0ea1d32840aab9b9837366dd4171 |
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| 出典メモ | uspto-grants-2015_05 |
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