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Sodium Iodide → 1-(4-chlorobenzyl)-5-(4-fluorophenoxy)pyridin-2(1H)-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | 1-Chloro-4-(chloromethyl)benzene | HCID 7723 | — |
| 反応物 | 5-(4-Fluorophenoxy)-2-methoxypyridine | HCID 44254192 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 1-(4-chlorobenzyl)-5-(4-fluorophenoxy)pyridin-2(1H)-one | HCID 58966921 | 27% |
反応手順
According to Scheme 32 Step 1: 5-(4-Fluorophenoxy)-2-methoxypyridine (2.37 mmol, 520 mg), 4-chlorobenzylchloride (3.55 mmol, 603 mg), NaI (2.37 mmol, 356 mg) in acetonitrile (15 mL) was heated at 150° C. for 20 minutes under microwave conditions. The cooled crude reaction washed with water, extracted with AcOEt. The organic layer was collected, dried (Na2SO4) and the solvent was evaporated under reduced pressure. The residue was purified in a manifold (vac.) using a Sep-Pak silica cartridge (heptane/AcOEt, 90:10 to CH2Cl2) and then CH2Cl2/acetone 90:10), following HPLC purification yielding 1-(4-chlorobenzyl)-5-(4-fluorophenoxy)pyridin-2(1H)-one (211 mg, 27%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08399493B2 |
| 出典データセット | uspto-grants-2013_03 |
| ORD ID | ord-8be4dd2a51f44dc6a36bff4fdc097106 |
| 出典メモ | uspto-grants-2013_03 |