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Sodium dichromate dihydrate → 8-Methylphenanthrene-1,10-dicarboxylic Anhydride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium dichromate dihydrate | HCID 108005 | — |
| 反応物 | 7-Methylacephenanthrylene | HCID 14932039 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 8-Methylphenanthrene-1,10-dicarboxylic Anhydride | HCID 53791006 | 82.4% |
反応手順
A suspension of 7-methylacephenanthrylene (0.56 g, 2.59 mmol) and sodium dichromate dihydrate (2.70 g, 9.07 mmol) in glacial acetic acid (10 mL) was heated at reflux for 4 h. The reaction mixture was allowed to cool and the resulting solid was collected by suction filtration. The solid was dried to give 0.56 g (80%) of the anhydride: MS (CI) m/e (%) 263 (M+H+, 100); 1H NMR (DMSO-d6, 300 MHz) δ 9.55 (d, 1H, J=8.8 Hz), 9.04 (s, 1H), 8.89 (d, 1H, J=8.5 Hz), 8.55 (d, 1H, J=7.4 Hz), 7.75 (d, 1H, J=7.3 Hz), 2.87 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05416089 |
| 出典データセット | uspto-grants-1995_05 |
| ORD ID | ord-9d9be11513e849ea88d6217bb19e8c22 |
| 出典メモ | uspto-grants-1995_05 |