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4-Iodo-1-tritylimidazole → 3-Fluoro-4-(5-iodo-imidazol-1-ylmethyl)benzonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Iodo-1-tritylimidazole | HCID 618252 | — |
| 反応物 | 4-(Bromomethyl)-3-fluorobenzonitrile | HCID 2783149 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 3-Fluoro-4-(5-iodo-imidazol-1-ylmethyl)benzonitrile | HCID 58827215 | — |
反応手順
A mixture of 4-iodo-1-trityl-1H-imidazole (17.1 g, 39.2 mmol) and 4-bromomethyl-3-fluorobenzonitrile (9.65 g, 45.08 mmol) in 150 mL of dry acetonitrile is stirred at room temperature for 7 days. After concentration, the residue is mixed with methanol, and heated to reflux for 1.5 h. The solvent is subsequently removed and the residue is treated with 1M HCl (300 mL). The resulting suspension is filtered and the washed with HCl (1 M). The combined solution is adjusted to PH 9-10 by saturated NaHCO3 solution. The resulting precipitation is collected by filtration, dried in vacuum oven. MS (ESI) m/z (M+H) 328.1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08835646B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-00356ce0b93c4b9eb25ec3d05af4d485 |
| 出典メモ | uspto-grants-2014_09 |