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Phosphorus oxide (P4O10) → 5-Bromo-6,6'-dimethyl-2-pivaloyloxy-2',3',4'-trimethoxybenzophenone
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-Pivaloyloxy-5-bromo-6-methylbenzoic acid | HCID 23293234 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 5-Bromo-6,6'-dimethyl-2-pivaloyloxy-2',3',4'-trimethoxybenzophenone | HCID 22671373 | — |
反応手順
A mixture of 50A (6.3 g, 20 mmol), 3,4,5-trimethoxytoluene (3.83 g; 21 mmol), P2O5 (12.0 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 flash chromatography with petrol ethers/ethyl acetate (9:1 v/v) as eluent yielding the pure product as white crystals, 5.58 g, (58.2%).
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-3051db69995040959e004c7e42720296 |
| 出典メモ | uspto-grants-2000_10 |