関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 1-Bromo-2-Chloroethane | HCID 7849 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4,5-Diphenylimidazole | HCID 69588 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 54222598 | HCID 54222598 | 17.7% |
反応手順
Step 1): A solution of 4,5-diphenylimidazole (2.5 g, 11.3 mmol) in dry DMF (20 ml) was added to a suspension of NaH (0.33 g, 13.8 mmol) in dry DMF (5 ml) at 50° C. under nitrogen atmosphere. The reaction mixture was heated at 60° C. for 2 hours. After heating, the mixture was added dropwise to a solution of 1-bromo-2-chloroethane (4.9 g, 33.9 mmol) in dry DMF (30 ml) over 1 hour at 50° C. The reaction mixture was heated continuously at 40° C. for 5 hours, then poured into water and extracted with ethyl acetate. The organic layer was washed with water, dried (MgSO4) and concentrated. The precipitates were filtered off. The filtrate was concentrated. The residue was purified by column chromatography on silica gel (ethyl acetate and hexane) to give 1-(2-chloroethyl)-4,5-diphenylimidazole (17.7%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05872115 |
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| 出典データセット | uspto-grants-1999_02 |
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| ORD ID | ord-558393d498c0477db34afe62487478cb |
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| 出典メモ | uspto-grants-1999_02 |
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