関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 6-Bromo-2-naphthalenol | HCID 27144 | — |
| 反応物 | Chlorosuccinimide | HCID 31398 | — |
| 触媒 | Zirconium chloride (ZrCl4), (T-4)- | HCID 9856075 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 6-Bromo-1-chloronaphthalen-2-ol | HCID 22048159 | 95.4% |
反応手順
The synthesis of (S1-2) was carried out following the method described in Synlett, No. 18, 2837 (2005), wherein 29.9 g of N-chlorosuccinimide and 600 ml of dichloromethane were added to a reactor in nitrogen atmosphere and cooled to 0° C., 2.6 g of zirconium (IV) chloride was added, and then 50 g of 6-bromo-2-naphthol (S1-1) was added slowly. The reaction solution was heated to room temperature and stirred for 10 hours, then washed with saturated sodium bicarbonate solution and water, dried over magnesium sulfate, and distilled under a reduced pressure to remove the solvent. Recrystallization was carried out using a mixed solvent of toluene/heptane=1/1 (volumetric ratio) to obtain 55 g of 6-bromo-1-chloro-2-naphthol (S1-2).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07727417B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-8195caeae8504cdfb40a16fc4ca39ca5 |
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| 出典メモ | uspto-grants-2010_06 |
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