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Phosphorus oxide (P4O10) → 1-(6'-Methyl-2',3',4'-trimethoxybenzoyl)-2-methoxynaphthalene
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 | Methyl 2-methoxy-1-naphthoate | HCID 604022 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(6'-Methyl-2',3',4'-trimethoxybenzoyl)-2-methoxynaphthalene | HCID 15870898 | — |
反応手順
A mixture of 5B (2.02 g, 10 mmol), 3,4,5-trimethoxytoluene (1.82 g; 10 mmol), P2O5 (10.0 g) and dichloromethane is stirred at room temperature for 16 hours. Subsequently, the dichloromethane is distilled off and the residue is diluted with ethyl acetate. The organic phase is washed with water and concentrated. The residue is purified by column chromatography (petrol ethers:ethyl acetate, 8:2 v/v) and recrystallized from petrol ether:diisopropylether (1:1 v/v). The solid material is collected by vacuum filtration, washed with cold petrol ether:diisopropylether (1:1 v/v) and dried, yielding white crystals, 0.9 g, (24.6%) mp 72° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06001883 |
| 出典データセット | uspto-grants-1999_12 |
| ORD ID | ord-14eafedcae5a4def8b11fef508cb35a7 |
| 出典メモ | uspto-grants-1999_12 |