참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Trimethyl borate | HCID 8470 | — |
| 반응물 | Lithium diisopropylamide | HCID 2724682 | — |
| 반응물 | 1-Methyl-3-(trifluoromethyl)-1H-pyrazole | HCID 2780404 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 1-Methyl-3-(trifluoroMethyl)pyrazole-5-boronic acid | HCID 12056713 | — |
반응 단계
A solution of 1-methyl-3-trifluoromethylpyrazol (2 g) in 10 ml THF is cooled under an inert gas atmosphere to −78° C. A 2 M solution of LDA (9.75 ml) is added dropwise. The mixture is stirred to 10° C. for 1 h and cooled to −75° C. Trimethylborate (5.8 ml) is added and after stirring for 1 h at −75° C. the mixture is stirred overnight at ambient temperature. The resulting reaction solution is added to 10% hydrochloric acid (15 ml). The water phase is extracted 3 times with ethyl acetate and the combined organic phases are washed with water and a saturated sodium chloride solution. The organic phase is dried and evaporated and the residue is crystallized from water. After drying, one obtains the title compound as nearly colorless crystals (1.12 g) of mp. 138° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06528456B2 |
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| 출처 데이터셋 | uspto-grants-2003_03 |
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| ORD ID | ord-b8b9c20b18d141b49324d4ebe17d2e8e |
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| 출처 메모 | uspto-grants-2003_03 |
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