関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | N-(hydroxymethyl)phthalimide | HCID 8354 | — |
| 反応物 | 5-methyl-2,4-dihydro-1H-3,1-benzoxazine-2,4-dione | HCID 10487522 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Methanesulfonic Acid | HCID 6395 | — |
| 生成物 | Phthalamide | HCID 6956 | 168.5% |
反応手順
To a solution of 5-methyl-4H-3,1-benzoxazin-2,4-dione (Preparation VIIA) (19.7 g, 111 mmol) in methanesulfonic acid (150 mL) was added N-(hydroxymethyl)phthalimide (20.3 g, 111 mmol). The reaction mixture was heated to 50° C. and stirred for 3 hours. After cooling to room temperature, the reaction mixture was diluted with 2000 mL of Et2O. After stirring for an additional 1 hour, the precipitate was filtered, washed with Et2O and dried affording 30.7 g of crude phthalamide. 1H NMR showed a 3:2 mixture of the 6- and 8-substituted regioisomers respectively. The crude material was used directly in the next reaction where the two regeoisomers were separated.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06380189B1 |
|---|
| 出典データセット | uspto-grants-2002_04 |
|---|
| ORD ID | ord-b24de7fa85a843819bcf06fc5284d1fb |
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| 出典メモ | uspto-grants-2002_04 |
|---|
