関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tributyltin Chloride | HCID 15096 | — |
| 反応物 | HCID 178418918 | HCID 178418918 | — |
| 反応物 | HCID 178505447 | HCID 178505447 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 6-fluoro-3-(tributylstannyl)-1H-indazole | HCID 178448232 | 106.9% |
反応手順
6-Fluoro-3-iodo-1H-indazole (300 mg, 1.1 mmol) in 30 mL of dry THF was cooled to −20° C. under nitrogen atmosphere, then isopropylmagnesium chloride (1.2 mL, 2.42 mmol) was added and mixture stirred for 15 mins at −20° C. Tributylchlorostannane (0.4 mL, 1.32 mmol) was added and the reaction mixture was allowed to warm to room temperature and stirred for 1 h. The reaction was quenched with saturated ammonium chloride, product extracted with ethyl acetate (3×50 mL), dried with sodium sulphate, filtered and concentrated to give 6-fluoro-3-(tributylstannyl)-1H-indazole (500 mg, crude) as a colorless oil which was used directly in the next step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08658646B2 |
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| 出典データセット | uspto-grants-2014_02 |
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| ORD ID | ord-29cd64a8d8eb4cdda7c870258d170685 |
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| 出典メモ | uspto-grants-2014_02 |
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