참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Trityl chloride | HCID 6456 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | HCID 178505409 | HCID 178505409 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 5-Bromo-6-fluoro-3-iodo-1-trityl-1H-indazole | HCID 68930723 | 73.9% |
반응 단계
To a solution of 3.0 g of 5-bromo-6-fluoro-3-iodo-1H-indazole in N,N-dimethylformamide in 150 mL was added 0.42 g of sodium hydride at room temperature, and the resultant solution was stirred for 15 minutes, added with 2.45 g of trityl-chloride, and stirred at this temperature for 1 hour. After adding water and diluting with ethyl acetate, washing successively with aqueous ammonium chloride and saturated brine and drying over anhydrous magnesium sulfate, the solvent was evaporated. The residue was purified and separated by silica gel column chromatography (ethyl acetate:n-hexane=1:30-1:5), and the resultant product was added with n-hexane. Then the precipitated crystals were washed with diethyl ether:n-hexane=1:10, to afford 3.79 g of the title compound as colorless crystals.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07429609B2 |
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| 출처 데이터셋 | uspto-grants-2008_09 |
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| ORD ID | ord-b36d63a95e0e48d082f464e0c9f219c6 |
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| 출처 메모 | uspto-grants-2008_09 |
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