関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Anisole | HCID 7519 | — |
| 反応物 | 2,6-Naphthalenedicarbonyl dichloride | HCID 3485596 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Nitrobenzene | HCID 7416 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | 2,6-Bis(4-methoxybenzoyl)naphthalene | HCID 19891124 | — |
反応手順
A stirred reactor comprising a 750 ml sulfonation flask, thermometer, condenser and nitrogen inlet is charged with 25.3 g (0.1 mol) of naphthalene-2,6-dicarbonyl dichloride and 32.4 g (0.2 mol) of anisole in 200 ml of nitrobenzene and, with stirring, 26.6 g (0.2 mol) of aluminium chloride are added over 15 minutes at 12°-18° C. The reaction mixture is thereafter allowed to react for 90 minutes at 40° C., then cooled to room temperature and thoroughly mixed with 1.5 liters of water containing HCl. The resultant suspension is diluted with 1.2 liters of N-methylpyrrolidone, and the mixture is heated to 130° C. The clear solution so obtained is cooled and the crystallised product is isolated by filtration. The filter residue is vacuum dried at 130° C., giving 25.9 g (65.4% of theory) of the desired product, which melts at 251° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05126427 |
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| 出典データセット | uspto-grants-1992_06 |
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| ORD ID | ord-40084545ddf24c55ab86285f440d97f2 |
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| 出典メモ | uspto-grants-1992_06 |
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