참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | N-Iodosuccinimide | HCID 120273 | — |
| 반응물 | 5-Bromo-6-fluoro-1H-indazole | HCID 46863923 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | HCID 178505409 | HCID 178505409 | 91.5% |
반응 단계
To a solution of 10.0 g of 5-bromo-6-fluoro-1H-indazole in 150 mL of N,N-dimethylformamide was added 10.5 g of N-iodosuccinimide at room temperature, and stirred at 70° C. for 2 days. Then the solution was diluted with ethyl acetate, washed successively with aqueous ammonium chloride and saturated brine, dried over anhydrous magnesium sulfate, and the solvent was evaporated. The crystals precipitated by adding diethyl ether to the residue were collected by filtration. The filtrate was further concentrated and purified and separated by silica gel column chromatographsy (ethyl acetate:n-hexane=1:10-1:5) and combined with the previous crystals, to afford 14.5 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-a8cb828c57634091a7280e761e4badb3 |
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| 출처 메모 | uspto-grants-2008_09 |
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