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2-Methylimidazole → 3-Bromo-5-(2-methyl-imidazol-1-ylmethyl)-pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Methylimidazole | HCID 12749 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 3-Bromo-5-(chloromethyl)pyridine | HCID 11701259 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3-Bromo-5-(2-methyl-imidazol-1-ylmethyl)-pyridine | HCID 23444965 | 53% |
反応手順
To a stirred suspension of sodium hydride (0.54 g, 12.3 mmol) in THF (40 ml) at 20° C. was added 2-methylimidazole in portions over 45 min. 3-Bromo-5-(chloromethyl)-pyridine (1 g, 4.1 mmol) in ethanol (8 ml) was then added and this mixture was heated under reflux for 1 h under an argon atmosphere. After cooling and evaporation of solvents the residue was suspended in MeOH, filtered and adsorbed onto silica gel. Chromatographic elution with CH2Cl2/(2M NH3 MeOH)=98:2 afforded the title compound (0.56 g, 53%) as a yellow oil. MS: m/e=251.0 (M+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06667335B2 |
| 出典データセット | uspto-grants-2003_12 |
| ORD ID | ord-c133a101e6df4d2bac17551362b8de36 |
| 出典メモ | uspto-grants-2003_12 |