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Formamide → 4-Methoxyisoindoline-1,3-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Formamide | HCID 713 | — |
| 反応物 | 4-Methoxy-1,3-dihydro-2-benzofuran-1,3-dione | HCID 291193 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-Methoxyisoindoline-1,3-dione | HCID 16638228 | 37% |
反応手順
A mixture of 3-methoxyphthalic anhydride (24.0 g, 134.8 mmol) and formamide (120 ml) was stirred and held at 210° C. for 5 hours and was then allowed to cool to room temperature overnight. Water (100 ml) was added and the solid material filtered off under reduced pressure. The crude product was washed sequentially with 50% aqueous acetone (50 ml) and diethyl ether (200 ml) and sucked dry under reduced pressure to afford 3-methoxyphthalimide (8.95 g, 37%) as an off-white solid. 1H NMR (DMSO-d6) 11.08 (1H, br s), 7.78 (1H, dd), 7.45 (1H, d), 7.36 (1H, d), 3.93 (3H, s). MS: [M+H]+ 178.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08101648B2 |
| 出典データセット | uspto-grants-2012_01 |
| ORD ID | ord-72be81a7801c49fd89559a9f8c568ae4 |
| 出典メモ | uspto-grants-2012_01 |