참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrogen Bromide | HCID 260 | — |
| 반응물 | Acetonitrile | HCID 6342 | — |
| 반응물 | 2-Amino-3-fluorobenzoic acid | HCID 586408 | — |
| 반응물 | Sodium Nitrite | HCID 23668193 | — |
| 촉매 | copper(I) bromide | HCID 24593 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 2-Bromo-3-fluorobenzoic acid | HCID 302622 | 100% |
반응 단계
In a 1 L, three necked flask fitted with a dropping funnel and thermometer, were charged 2-amino-3-fluorobenzoic acid (20.0 g, 0.13 mol) and acetonitrile (160 mL). After cooling to 0° C., HBr (47%, 160 mL) was added drop wise over 10 min. To the resulting solution a solution of NaNO2 (10.0 g, 0.14 mol) in water (20.0 mL) was added drop wise over 1 h. After addition, the reaction mixture was stirred at 0° C. for 5 min, and copper(I) bromide (22.0 g, 0.15 mol) was added portionwise over 30 min. Stirring was continued at 70° C. in a an oil bath for 1 h. After cooling to 0° C., 700 mL of water was added and the precipitate was filtered, washed with cold water and dried under vacuum to give 28.23 g (100%) of the title compound as a white solid. The crude product was used in the next step without purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08633186B2 |
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| 출처 데이터셋 | uspto-grants-2014_01 |
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| ORD ID | ord-b7e4cabab20244c384a9c5b988e858d5 |
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| 출처 메모 | uspto-grants-2014_01 |
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