関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tributyltin Chloride | HCID 15096 | — |
| 反応物 | 1H-Pyrazole, 1-methyl- | HCID 70255 | — |
| 反応物 | Lithium diisopropylamide | HCID 2724682 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-Methyl-5-(tributylstannyl)-1H-pyrazole | HCID 21867455 | — |
反応手順
Lithium diisopropylamide (1.5 M in cyclohexane) (9.7 mL, 14.6 mmol) was added to a −78° C. solution of 1-methylpyrazole (1 g, 12.2 mmol) in tetrahydrofuran (15 mL). After stirring at −78° C. for 15 min, chloro-tri-n-butylstannane (3.9 mL, 14.6 mmol) was added dropwise. The reaction mixture was allowed to warm to ambient temperature overnight. The reaction mixture was quenched with saturated aqueous ammonium chloride, diluted with water and extracted with ethyl acetate. The combined organic extracts were dried (magnesium sulfate), filtered and concentrated in vacuo. Chromatography over silica eluting with 0-100 ethyl acetate/hexane afforded 1-methyl-5-(tributylstannyl)-1H-pyrazole.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08193228B2 |
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| 出典データセット | uspto-grants-2012_06 |
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| ORD ID | ord-8314bb2997214012b96ae829d21c7b06 |
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| 出典メモ | uspto-grants-2012_06 |
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