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Diethyl (ethoxymethylene)malonate → (S)-Diethyl (7,8-Difluoro-3-Methyl-3,4-Dihydro-2H-[1,4]Benzoxazin-4-Yl)Methylene-Malonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethyl (ethoxymethylene)malonate | HCID 6871 | — |
| 反応物 | (3S)-3-Methyl-7,8-difluoro-2,3-dihydro-4H-1,4-benzoxazine | HCID 11041424 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | (S)-Diethyl (7,8-Difluoro-3-Methyl-3,4-Dihydro-2H-[1,4]Benzoxazin-4-Yl)Methylene-Malonate | HCID 11089557 | 88% |
反応手順
To DMF (2.5 ml) was added potassium tertiary-butoxide (75 mg) under ice-cooling. After dropping a solution of the compound (100 mg) obtained in Example 78 and diethyl ethoxymethylenemalonate (233 mg) in DMF (0.5 ml), the resultant mixture was stirred for 2 hours. After treating in a conventional manner, the obtained residue was subjected to silica gel column chromatography to thereby give 153 mg (88%) of the title compound as an oily product. The physical constants of the obtained compounds was identical with those described in Japanese Patent No. 2,769,174.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07087778B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-4eb0b563d26541c38317838c6ee3f3f4 |
| 出典メモ | uspto-grants-2006_08 |