참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 1,2-Difluorobenzene | HCID 9706 | — |
| 반응물 | Triisopropyl borate | HCID 21531 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | (2,3-Difluorophenyl)boronic acid | HCID 2734333 | 86.7% |
반응 단계
After 7.5 g of o-difluorobenzene was dissolved in 80 ml of dried tetrahydrofuran (THF), the solution thus formed was cooled down to -70° C. under a nitrogen atmosphere and then added dropwise with 42 ml of butyllithium (1.6 mol/liter hexane solution) at a temperature lower than -55° C. The solution was continuously stirred at the same temperature for 1.5 hours and added dropwise with a THF solution containing 24.8 g of triisopropylborate at a temperature of -65° C. to -60° C. After the dropping of the solution was finished, the solution was continuously stirred at an ambient temperature for 12 hours, added further with 60 ml of a 10% aqueous hydrochloric acid solution, and continuously stirred for 1 hour. The reaction mixture thus obtained was subjected to extraction with an ether, washed with water, dried, and subjected to distillation under a reduced pressure to separate the solvent to obtain 9.0 g of 2,3-difluorophenyl boronic acid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05417885 |
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| 출처 데이터셋 | uspto-grants-1995_05 |
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| ORD ID | ord-5c1fdac029a140588c1ba6d6fc5c9073 |
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| 출처 메모 | uspto-grants-1995_05 |
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