참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Trimethyltin chloride | HCID 14016 | — |
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | 5-Bromo-4-chloro-7H-pyrrolo[2,3-d]pyrimidine | HCID 5380710 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 5-(Trimethylstannyl)-4-chloro-7H-pyrrolo[2,3-d]pyrimidine | HCID 11461236 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07323453B2 |
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| 출처 데이터셋 | uspto-grants-2008_01 |
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| ORD ID | ord-3a54b8808b9645c2a9df29a1b12740b8 |
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| 출처 메모 | uspto-grants-2008_01 |
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