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2-Bromo-1-(3,4-dichlorophenyl)ethanone → HCID 178477975、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Bromo-1-(3,4-dichlorophenyl)ethanone | HCID 244751 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| 反応物 | 6-Chloro-3-pyridinecarbonitrile | HCID 5152094 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 178477975 | HCID 178477975 | — |
反応手順
Lithium hexamethyldisilazide (41.5 mL of a 1.0 M solution in THF) was added to a solution of 2-chloro-5-cyanopyridine (5.24 g) in THF (10 mL). The resultant mixture was stirred at room temperature for 30 min, and then 13 mL saturated aqueous sodium bicarbonate and 5 mL water were added to the reaction mixture. A solution of 3,4-dichlorophenacyl bromide (10.13 g) in chloroform (150 mL) was added in two portions approximately 15 min apart. The resultant mixture was stirred for 72 hours, and the reaction mixture was filtered. The filter cake was triturated with dichloromethane (50 mL) to provide 2-Chloro-5-[4-(3,4-dichloro-phenyl)-1H-imidazol-2-yl]-pyridine (10.46 g). MS m/z 324 (M+), 326 (M++2).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06355635B1 |
| 出典データセット | uspto-grants-2002_03 |
| ORD ID | ord-ee9b6e165ef34b6fb9cf15324b2925e1 |
| 出典メモ | uspto-grants-2002_03 |