関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tributyltin Chloride | HCID 15096 | — |
| 反応物 | 5-((tert-Butyldimethylsilyl)oxy)-3-iodo-1-methyl-1H-indazole | HCID 71279866 | — |
| 反応物 | HCID 178418918 | HCID 178418918 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 5-(tert-butyldimethylsilyloxy)-1-methyl-3-(tributylstannyl)-1H-indazole | HCID 71279605 | 94.3% |
反応手順
The solution of 5-(tert-butyldimethylsilyloxy)-3-iodo-1-methyl-1H-indazole (3.8 g, 10 mmol) in 30 mL of dry THF was cooled to −20° C. under nitrogen, isopropylmagnesium chloride (6 mL, 12 mmol, 2M in THF) was added and stirred for 15 min at −20° C. Tributylchlorostannane (12 mL, 14 mmol) was added and the reaction mixture was allowed to warm to room temperature and stirred for 1 h. The mixture was quenched with saturated solution of ammonium chloride, extracted with ethyl acetate (3×50 mL), dried over sodium sulfate and concentrated to give 5-(tert-butyldimethylsilyloxy)-1-methyl-3-(tributylstannyl)-1H-indazole (5.2 g, crude) as a colourless 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-3d960b5cf7474d26b5e0fba2c9e1ffa1 |
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| 出典メモ | uspto-grants-2014_02 |
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