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Phosphorus oxide (P4O10) → 2-Acetoxy-5-bromo-6,6'-dimethyl-2', 3', 4'-trimethoxy-benzophenone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phosphorus oxide (P4O10) | HCID 14812 | — |
| 反応物 | 3,4,5-Trimethoxytoluene | HCID 80922 | — |
| 反応物 | 2-Acetoxy-5-bromo-6-methylbenzoic acid | HCID 11011149 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Acetoxy-5-bromo-6,6'-dimethyl-2', 3', 4'-trimethoxy-benzophenone | HCID 10906251 | — |
反応手順
A mixture of 1C (6.83 g, 25 mmol), 3,4,5-trimethoxytoluene (4.56 g; 25 mmol), P2O5 (15.0 g) and dichloromethane (100 ml) is stirred at room temperature for 16 hours. Subsequently, the dichloromethane is distilled off and the residue is diluted with water and ethyl acetate. The organic phase is washed with water and concentrated. The residue is purified by preparative HPLC with acetonitrile:water 9:1 as eluent yielding the pure product as a yellow oil, 1.1 g, (10.1%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06127570 |
| 出典データセット | uspto-grants-2000_10 |
| ORD ID | ord-4dc664032bb44c57911b3f9aacc56af6 |
| 出典メモ | uspto-grants-2000_10 |