関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2,4,5-Tribromoimidazole | HCID 16253 | — |
| 反応物 | 2-Chloromethyl 2-(trimethylsilyl)ethyl ether | HCID 2724271 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2,4,5-tribromo-1-[[2-(trimethylsilyl)ethoxy]methyl]-1H-Imidazole | HCID 10906203 | 83% |
反応手順
To a solution of 2,4,5-tribromoimidazole (3.05 g, 10 mmol) in anhydrous DMF (50 mL) was added powdered K2CO3 (19 g, 137 mmol), and the resulting suspension was stirred vigorously and treated dropwise with SEMCl (2.3 g, 13.8 mmol). The suspension was then stirred vigorously overnight. The solid was filtered off and washed with fresh DMF (20 mL). The combined filtrates were then evaporated under reduced pressure. Methylene chloride (30 mL) was then added and the solution washed with 0.1 N Na2CO3 (3×50 mL), dried (Na2SO4), filtered and evaporated to give a residue, which was passed through a silica gel pad (CH2Cl2) and evaporated to give 3.6 g (83%) of the title compound as a colorless oil. 1H NMR (500 MHz, CDCl3) δ 0.01 (s, 9H), 0.93 (t, 2H, J=8.0 Hz), 3.60 (t, 2H, J=8.0 Hz), 5.32 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07348425B2 |
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| 出典データセット | uspto-grants-2008_03 |
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| ORD ID | ord-25b81ac297f4471fb565d9435e82fe74 |
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| 出典メモ | uspto-grants-2008_03 |
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