関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4-Fluorobenzylic alcohol | HCID 68022 | — |
| 反応物 | 7-Fluoroquinazolin-4(3H)-one | HCID 135398496 | — |
| 反応物 | 7-(4-Fluoro-benzyloxy)-3H-quinazolin-4-one | HCID 135752715 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-[7-(4-Fluoro-benzyloxy)-4-oxo-4H-quinazolin-3-yl]-acetamide | HCID 10087813 | 66% |
反応手順
7-(4-Fluoro-benzyloxy)-3H-quinazolin-4-one: A mixture of sodium hydride (55%, 3.2 g, 73 mmol), 4-fluorobenzyl alcohol (9.2 g, 73 mmol) and 7-fluoro-3H-quinazolin-4-one (3.0 g, 18 mmol) in DMF (75 mL) was heated at 140° C. for 2 h. The resulting suspension was cooled to rt and the mixture acidified to pH 3 with HCl (conc.). The resulting precipitate was then filtered off, washed with water and diethylether. Partial purification by chromatography on silica gel eluting with ethyl acetate:hexane (2:1) afforded the title compound (3.2 g, 66%) as an off-white solid. MS: m/e=271.3 (M+H+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07087612B2 |
|---|
| 出典データセット | uspto-grants-2006_08 |
|---|
| ORD ID | ord-02ebb08f2555436889139e7598c8df89 |
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| 出典メモ | uspto-grants-2006_08 |
|---|
