関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,4-Dichlorophthalazine | HCID 78490 | — |
| 反応物 | 7-Methoxy-2-naphthol | HCID 853173 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | 1-(4-Chlorophthalazin-1-yl)-7-methoxynaphthalen-2-ol | HCID 136343453 | 80% |
反応手順
In a 1 L flask under nitrogen were mixed 1,4-dichlorophthalazine (11.4 g, 57.3 mmol) with 7-methoxy-naphthalen-2-ol (10.0 g, 57.5 mmol). To this was added 1,2-dichloroethane (450 ml). After stirring for 10 min, aluminum chloride (7.64 g, 57.4 mmol) was added. The resulting suspension was stirred for 20 hrs at 80° C. After cooling to room temperature, the black suspension was poured on ice-water (500 ml) and stirred for 1 hr. The two layers were separated. The aqueous layer was extracted with dichloromethane (3×200 ml). The combined organic layers were dried over sodium sulfate and concentrated under reduced pressure. The crude solid was triturated with dichloromethane (35 ml) for 1 hr and collected by filtration to give 15.2 g of the title compound as a grey solid. (Yield: 80%)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07790882B2 |
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| 出典データセット | uspto-grants-2010_09 |
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| ORD ID | ord-ed23b821dc2e4ab4985a78b5a2f88016 |
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| 出典メモ | uspto-grants-2010_09 |
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