참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Methyl trifluoroacetate | HCID 9893 | — |
| 반응물 | 4-Bromo-2,6-difluoroanisole | HCID 2773287 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 1-(3,5-Difluoro-4-methoxyphenyl)-2,2,2-trifluoroethanone | HCID 86722578 | 100.3% |
반응 단계
Isopropyl magnesium chloride lithium chloride complex (22.0 mL, 28.02 mmol) was added dropwise to a stirred solution of 5-bromo-1,3-difluoro-2-methoxybenzene (5.0 g, 22.42 mmol) at −5° C. in THF (100 mL) and the reaction mixture was stirred at same temperature for 30 min. Methyl trifluoroacetate (3.67 g, 28.69 mmol) was added dropwise and the reaction mixture was stirred at ambient temperature for 2 h. A 2 N HCl solution (200 mL) was added to quench the reaction and then it was extracted with diethylether. The combined organic layers were washed with brine, dried (Na2SO4) filtered and concentrated to afford the title compound (5.4 g, crude) as a yellow liquid. The material was taken to next step without further purification. 1H NMR (400 MHz, CDCl3) δ 7.68-7.60 (m, 2H) 4.19 (s, 3H); ESIMS m/z 240.1 ([M]+).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09226501B2 |
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| 출처 데이터셋 | uspto-grants-2016_01 |
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| ORD ID | ord-c941b14a50a14027819f3d5381de4a3c |
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| 출처 메모 | uspto-grants-2016_01 |
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