関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | 2-Amino-6-fluorobenzoic acid | HCID 521142 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 6-Amino-3-bromo-2-fluorobenzoic acid | HCID 67080905 | 50% |
反応手順
To a solution of 2-amino-6-fluorobenzoic acid (12.0 g, 77.35 mmol) in methanol (150 mL) was added bromine (15.7 mL) at −78° C., and the mixture was stirred 2 hours at −78° C. The reaction mixture was quenched with ice-water (100 mL) and aqueous solution of sodium sulfothioate, and extracted with ethyl acetate (150 mL×3). The organic layers were separated, combined, washed with water (100 mL) and brine (100 mL), dried over sodium sulfate, filtered and concentrated to afford the title crude product (9.0 g, 50%). MS (ES+) C7H5BrFNO2 requires: 232, found: 233, 235 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09434700B2 |
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| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-3be058ae97094217b22ec234aab109a0 |
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| 出典メモ | uspto-grants-2016_09 |
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