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Sodium hydride → 2-n-butyl-1-(2-chloro-6-fluorophenyl)methyl-1H-imidazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 1-Chloro-2-(chloromethyl)-3-fluorobenzene | HCID 108675 | — |
| 反応物 | 2-butyl-1H-imidazole | HCID 11815351 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-n-butyl-1-(2-chloro-6-fluorophenyl)methyl-1H-imidazole | HCID 19936774 | 95.3% |
反応手順
A solution of 2 n-butylimidazole (3.75 g, 0.03 mol) in dry dimethylformamide (4 ml) was added to sodium hydride (0.95 g) in dimethylformamide (18 ml). After the gas evolution subsided, the mixture was stirred one hour under argon and 2-chloro-6-fluorobenzylchloride (5.5 q, 0.031 mol) in dimethylformamide (7 ml) was added slowly. The mixture was stirred for 17 hours at ambient temperature, diluted with ice water and extracted with ethyl acetate. The washed, dried, concentrated organic layer provided 7.63 g (94%) of 2-n-butyl-1-(2-chloro-6-fluorophenyl)methyl-1H-imidazole whose NMR was consistent with the structure. This material was used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05248689 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-bc86844699a84905a340fdf779a0e7ca |
| 出典メモ | uspto-grants-1993_09 |