関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Trimethyltin chloride | HCID 14016 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 5-Bromo-4-chloro-7H-pyrrolo[2,3-d]pyrimidine | HCID 5380710 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 5-(Trimethylstannyl)-4-chloro-7H-pyrrolo[2,3-d]pyrimidine | HCID 11461236 | — |
反応手順
To a solution of the compound from Step A (0.92 g, 4 mmol) in THF (25 mL) was added n-BuLi (2.5 M solution in hexane, 3.48 mL) dropwise at −78° C. After the addition, the reaction mixture was stirred at −78° C. for an additional 30 min. To this solution was added trimethyltin chloride (0.88 g, 4.4 mmol) in THF (8 mL) dropwise for a period of 10 min. The reaction mixture was brought to room temperature slowly and stirred at room temperature overnight. Saturated aqueous ammonium chloride (60 mL) was added and extracted with ethyl acetate (3×70 mL). The combined organic extracts were washed with brine, dried over Na2SO4 and evaporated to dryness. The residue was purified over silica gel to give the title compound as a colorless solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07323453B2 |
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| 出典データセット | uspto-grants-2008_01 |
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| ORD ID | ord-3a54b8808b9645c2a9df29a1b12740b8 |
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| 出典メモ | uspto-grants-2008_01 |
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