참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ammonia | HCID 222 | — |
| 반응물 | Potassium Fluoride | HCID 522689 | — |
| 반응물 | (Trifluoromethyl)trimethylsilane | HCID 552549 | — |
| 반응물 | 5-Bromo-2-iodopyrimidine | HCID 7006651 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 생성물 | 5-Bromo-2-(trifluoromethyl)pyrimidine | HCID 33697963 | — |
반응 단계
A mixture of potassium fluoride (1.77 g) and cuprous iodide (5.79 g) was stirred and heated together using a heat gun under vacuum (˜1 mm) for 20 min. After cooling, dimethyl formamide (20 ml) and N-methylpyrrolidinone (20 ml) were added followed by (trifluoromethyl)trimethylsilane (4.1 ml) and 5-bromo-2-iodopyrimidine (6.5 g). The mixture was stirred at rt for 5 h and then the brown solution was poured into 6N ammonia solution. The product was extracted into ethyl acetate and the extracts were washed with sodium bicarbonate solution and brine and then dried (Na2SO4) and evaporated. Chromatography on silica gel (elution with 20-50% dichloromethane in pentane) gave the title compound (D13) as a white solid (2.4 g). 1H NMR (CDCl3): 8.97 (2H, s).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08492375B2 |
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| 출처 데이터셋 | uspto-grants-2013_07 |
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| ORD ID | ord-5a9c459d47ab462eb3a52a66414054c5 |
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| 출처 메모 | uspto-grants-2013_07 |
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