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Acetic Anhydride → 4-Methoxy-1,3-dihydro-2-benzofuran-1,3-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | 3-Methoxyphthalic acid | HCID 315218 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-Methoxy-1,3-dihydro-2-benzofuran-1,3-dione | HCID 291193 | 99.1% |
反応手順
Acetic anhydride (70 ml) was added to a mixture of 3-methoxyphthalic acid (51.0 g, 0.26 mol) in anhydrous tetrahydrofuran (250 ml) and the mixture was stirred and held at reflux for 4 hours. Upon cooling to room temperature the solvent was removed in vacuo and the resulting solid material was dried in a vacuum oven at 50° C. overnight to afford 3-methoxyphthalic anhydride (45.9 g, 99%) as a colourless solid. 1H NMR (DMSO-d6) 7.97 (1H, dd), 7.63 (1H, d), 7.60 (1H, d), 4.02 (3H, s). MS: [M+H]+ 179.
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-9395b52f44e0434d8de65dec1c770de9 |
| 出典メモ | uspto-grants-2012_01 |