関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Boron tribromide | HCID 25134 | — |
| 反応物 | 7-Methoxyisoquinoline | HCID 594375 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 7-Isoquinolinol | HCID 459767 | 80.6% |
反応手順
To a 2-liter, 3-necked round bottom flask equipped with a magnetic stir bar and addition funnel is added 19.7 g (0.124 mole) 7-methoxyisoquinoline and 800 ml of dry dichloromethane. This solution is stirred and cooled to -75° C. with a dry ice/acetone bath, 628 ml (0.628 mole) of 1.0M boron tribromide in dichloromethane is added dropwise maintaining the temperature at -75° C. Thereafter the slurry is stirred for 18 hours allowing the temperature to rise to room temperature. The reaction slurry is poured into 1 liter of ice water and stirred for an hour. The layers are separated and the aqueous layer is then adjusted from acidic to neutral (pH 7) with 1N NaOH. A yellow solid precipitates and is filtered off, then air dried to yield 14.5 g of a yellow solid, 81%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05770586 |
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| 出典データセット | uspto-grants-1998_06 |
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| ORD ID | ord-127741b5bb1c45bdace07f5900d2d152 |
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| 出典メモ | uspto-grants-1998_06 |
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