関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Ethyl chloronicotinate | HCID 2796614 | — |
| 反応物 | HCID 178418822 | HCID 178418822 | — |
| 触媒 | 18-Crown-6 | HCID 28557 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Ethyl 2-(4-phenyl-1H-imidazol-1-yl)pyridine-3-carboxylate | HCID 66720067 | 28.9% |
反応手順
A mixture of 5.0 g of ethyl 2-chloronicotinate (26.94 mmol), 3.4 g of 4-phenylimidazole (23.58 mmol), 7.6 g of K2CO3 and 80 mg of 18-crown-6 in 18 ml of N,N-dimethylformamide was heated in a microwave at 160° C. for about 1 hour. This was followed by concentrating, taking up the residue in dichloromethane, washing with water and sat. NaCl solution, drying over MgSO4, filtering and evaporating. Chromatography on silica gel (eluent: CH2Cl2/methanol 2%-5%) resulted in 2 g of a dark oil, which was immediately reacted further; ESI-MS [M+H]+=294.15.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07799809B2 |
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| 出典データセット | uspto-grants-2010_09 |
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| ORD ID | ord-a1e1edc5433c4c4685f92df7f0b6d707 |
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| 出典メモ | uspto-grants-2010_09 |
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