関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | 2-Amino-4-methylbenzamide | HCID 2801474 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | 5-(4-Fluorophenyl)-1,3-dioxolane-2,4-dione | HCID 86649050 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-[(4-fluorophenyl)-hydroxymethyl]-7-methyl-1H-quinazolin-4-one | HCID 178422980 | 91% |
反応手順
To a solution of 2-amino-4-methylbenzamide (3 g, 20.0 mmol) in THF (40 mL) was added 5-(4-fluorophenyl)-1,3-dioxolane-2,4-dione from Example 16 (4.7 g, 24 mmol) and the solution was stirred for 2 h at 50° C. Sodium methoxide in MeOH (25%, 5.2 mL, 24 mmol) was then added and the solution was stirred at 50° C. overnight. The reaction mixture solution was concentrated, 2N HCl was added and the mixture was filtered. The collected solid was dried to give 2-(((4-fluorophenyl)(hydroxy)methyl)-7-methylquinazolin-4-ol (5.14 g, 91%) which was used without further purification. LC-MS (ESI) m/z 285 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09308207B2 |
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| 出典データセット | uspto-grants-2016_04 |
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| ORD ID | ord-4b4408a992bb4972b29016de0773ca8e |
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| 出典メモ | uspto-grants-2016_04 |
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