関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Ethane, 1-chloro-2-ethoxy- | HCID 12341 | — |
| 反応物 | 2-Chlorobenzimidazole | HCID 78572 | — |
| 反応物 | Potassium bis(trimethylsilyl)amide | HCID 3251421 | — |
| 触媒 | Tetrabutylammonium Bromide | HCID 74236 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-chloro-1-(2-ethoxyethyl)-1H-benzimidazole | HCID 10489356 | — |
反応手順
Combine 2-chloro-1H-benzimidazole (15.3 g, 100 mmol) and tetrahydrofuran (300 mL). Cool to −70° C. Add dropwise, a solution of potassium bis(trimethylsilyl)amide (200 mL, 0.5 M in toluene, 100 mmol). After 30 minutes, add 2-chloroethyl ethyl ether (22.2 g, 200 mmol) and tetrabutylammonium bromide (0.5 g). Warm to ambient temperature and heat to reflux. After 12 hours, cool to ambient temperature and add water. Separate the organic layer and extract the aqueous layer with dichloromethane. Dry the combined organic layers over Na2SO4, filter, and evaporate in vacuo to give 1-(2-ethoxyethyl)-2-chloro-1H-benzimidazole.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06211199B1 |
|---|
| 出典データセット | uspto-grants-2001_04 |
|---|
| ORD ID | ord-403afb8cca9e4aef927dd4122a2a3c3e |
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| 出典メモ | uspto-grants-2001_04 |
|---|
