化工社化工社 化学情報印刷レポート · 研究参考用
Dicyclohexylcarbodiimide → 6-(1-Imidazolylmethyl)benzoxazol-2-yl-methyl methyl 1,4-dihydro-2,6-dimethyl-4-(3-nitrophenyl)pyridine-3,5-dicarboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dicyclohexylcarbodiimide | HCID 10868 | — |
| 反応物 | 2,6-Dimethyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3,5-dicarboxylic acid monomethyl ester | HCID 173322 | — |
| 反応物 | 2-Hydroxymethyl-6-(1-imidazolylmethyl)benzoxazole | HCID 70047035 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 6-(1-Imidazolylmethyl)benzoxazol-2-yl-methyl methyl 1,4-dihydro-2,6-dimethyl-4-(3-nitrophenyl)pyridine-3,5-dicarboxylate | HCID 70048044 | — |
反応手順
332 mg (1 mM) of 1,4-dihydro-2,6-dimethyl-5-methoxycarbonyl-4-(3-nitrophenyl)pyridine-3-carboxylic acid together with 229 mg (1 mM) of 2-hydroxymethyl-6-(1-imidazolylmethyl)benzoxazole 248 mg (1.2 mM) of dicyclohexylcarbodiimide and 134 mg (1.1 mM) of 4-N,N-dimethylaminopyridine were dissolved in 5 ml of toluene, while heating, and refluxed for six hours. The solution was cooled to room temperature, and the crystals produced were filtered off. The filtrate was washed with water and dried over anhydrous sodium sulfate. After the solvent was distilled off, the residue was purified by chromatography on a silica gel column, whereby the captioned compound was obtained. The yield was 542 mg (99.9%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05286869 |
| 出典データセット | uspto-grants-1994_02 |
| ORD ID | ord-226a9f9367aa4ac39fbe3ddc55086a66 |
| 出典メモ | uspto-grants-1994_02 |