関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-Aminobenzoic Acid | HCID 7419 | — |
| 反応物 | Trifluoroacetic anhydride | HCID 9845 | — |
| 反応物 | 2-Oxo-2-phenylethyl 3-[(trifluoroacetyl)amino]benzoate | HCID 1159354 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-[(Trifluoroacetyl)amino]benzoic acid | HCID 283840 | — |
反応手順
A compound having general Formula 4, exemplified by 3-(2,2,2-Trifluoro-acetylamino)-benzoic acid 2-oxo-2-phenyl-ethyl ester (Compound 4; FIG. 1) can be prepared as follows. A solution of 3-aminobenzoic acid (137 mg, 1.0 mmol) in dichloromethane is treated with trifluoroacetic anhydride (420 mg, 2.0 mmol). The reaction mixture is stirred until no further reaction occurs. The reaction mixture is concentrated to give 3-(2,2,2-Trifluoro-acetylamino)-benzoic acid. A solution of 3-(2,2,2-Trifluoro-acetylamino)-benzoic acid (233 mg, 1.0 mmol) and 2-hydroxyacetophenone (136 mg, 1.0 mmol) in dimethylformamide and diisopropylethylamine (260 mg, 2.0 mmol) is treated with HBTU (379 mg, 1.0 mmol). The reaction mixture is stirred until no further reaction occurs. The reaction is poured into ethyl acetate and water. The organic phase is collected, dried and concentrated to give the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07728034B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-3c010eccc78f4f318379f1311a2a0e99 |
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| 出典メモ | uspto-grants-2010_06 |
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