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Sodium Methoxide → 2-[7-(3-Fluoro-benzyloxy)-2-methyl-4-oxo-4H-quinazolin-3-yl]-acetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | Ethyl acetamidate hydrochloride | HCID 19983589 | — |
| 反応物 | 2-Amino-4-(3-fluoro-benzyloxy)-benzoic acid | HCID 21991777 | — |
| 反応物 | 7-(3-Fluoro-benzyloxy)-2-methyl-3h-quinazolin-4-one | HCID 135752714 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-[7-(3-Fluoro-benzyloxy)-2-methyl-4-oxo-4H-quinazolin-3-yl]-acetamide | HCID 10020180 | 97% |
反応手順
7-(3-Fluoro-benzyloxy)-2-methyl-3H-quinazolin-4-one: To a mixture of 2-amino-4-(3-fluoro-benzyloxy)-benzoic acid (2.0 g, 7.7 mmol) and ethyl acetamidate HCl (1.9 g, 15.3 mmol) in methanol (30 mL) was added sodium methoxide (5.4 M, 0.83 g, 15.3 mmol) and the resulting mixture was heated under reflux for 19 h. After this time ethyl acetamidate HCl (1.9 g, 15.3 mmol) and sodium methoxide (5.4 M, 0.83 g, 15.3 mmol) was added and the resulting mixture heated for another 1 h. After cooling to rt the mixture was poured into water (40 mL) and then the resulting precipitate was stirred for 2 h, and filtered off to afford the title compound (2.1 g, 97%) as an off-white solid. MS: m/e=283.1 (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-b61c6f8fbaaa4529848801b75a7c15ca |
| 出典メモ | uspto-grants-2006_08 |