関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Lithium amide | HCID 24532 | — |
| 反応物 | 2,3,4-Trifluorobenzoic acid | HCID 302932 | — |
| 反応物 | 4-Bromo-2-chloroaniline | HCID 610169 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2-[(4-Bromo-2-chlorophenyl)amino]-3,4-difluorobenzoic acid | HCID 59469244 | 94% |
反応手順
To a solution of 2,3,4-trifluorobenzoic acid (1 g, 5.68 mmol) and 4-bromo-2-chloroaniline (1.2 g, 5.68 mmol) in acetonitrile (10 mL) was added lithium amide (0.39 g, 17.04 mmol) and the reaction stirred at 60° C. for 1.5 hours. The mixture was cooled to room temperature and then to 0° C. and acidified with aq. hydrochloric acid. The obtained precipitate was collected by filtration and washed with cold water and dried in vacuo to afford 2[(4-bromo-2-chlorophenyl)amino]-3,4-difluorobenzoic acid (1.92 g, 94% yield) as a beige solid. MS (EI) for C13H7BrClF2NO2: 363 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07915250B2 |
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| 出典データセット | uspto-grants-2011_03 |
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| ORD ID | ord-dd40e3c5df0e4ca0bd816e2ec05a3cf4 |
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| 出典メモ | uspto-grants-2011_03 |
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