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Water → 4,5-Bis(2-benzyloxyacetyloxy)-9,10-dioxo-9,10-dihydroanthracene-2-carboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Rhein | HCID 10168 | — |
| 反応物 | Benzyloxyacetyl chloride | HCID 177085 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 4,5-Bis(2-benzyloxyacetyloxy)-9,10-dioxo-9,10-dihydroanthracene-2-carboxylic acid | HCID 11455980 | — |
反応手順
4,5-Dihydroxy-9,10-dioxoanthracene-2-carboxylic acid (3.0 g) was suspended in pyridine (100 ml) and stirred at RT for 30 mins. Benzyloxyacetyl chloride (3.6 g, 5 equiv.) was added, to give a clear reaction mixture which was stirred at RT over the weekend. The reaction mixture was reduced to a smaller volume and quenched with 2M HCl (200 ml), adjusting the pH to pH 2. An orange solid was isolated by filtration. This crude solid was slurried in water (30 ml), followed by ethyl acetate (30 ml) and dichloromethane (30 ml). A yellow solid was isolated by filtration (3.6 g, 61%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07728035B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-ba0d0475fac4495ead26baa58c66eb98 |
| 出典メモ | uspto-grants-2010_06 |