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Hydrochloric Acid → 2-[7-(3-Fluoro-benzyloxy)-4-oxo-4H-quinazolin-3-yl]-acetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 3-Fluorobenzylic alcohol | HCID 68008 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 反応物 | 7-Fluoroquinazolin-4(3H)-one | HCID 135398496 | — |
| 反応物 | 7-(3-Fluoro-benzyloxy)-3H-quinazolin-4-one | HCID 135752716 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-[7-(3-Fluoro-benzyloxy)-4-oxo-4H-quinazolin-3-yl]-acetamide | HCID 9862180 | 61% |
反応手順
7-(3-Fluoro-benzyloxy)-3H-quinazolin-4-one: Sodium (1.8 g, 78.6 mmol) was added portionwise to 3-fluorobenzyl alcohol and the resulting mixture heated at 80–90° C. for 4 h under Argon. The resulting suspension was cooled to rt and 7-fluoro-3H-quinazolin-4-one (3.2 g, 19.5 mmol) was added and the resulting mixture heated at 130–140° C. for 14 h. The solid formed was then dissolved with water (400 mL) and the mixture acidified to pH 3–4 with HCl (4 N). The resulting precipitate was then filtered off, washed with water (100 mL) and diethylether (100 mL). Recrystallisation from tetrahydrofuran: ethylacetate (1:1) afforded the title compound (3.2 g, 61%) as white crystals. 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-af083bdcb1c9493f8949656570ce9951 |
| 出典メモ | uspto-grants-2006_08 |