関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Trifluoroacetic anhydride | HCID 9845 | — |
| 反応物 | 4-(Methylamino)benzoic acid | HCID 66345 | — |
| 反応物 | Benzoic acid, 4-[methyl(trifluoroacetyl)amino]- | HCID 10514620 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | Benzoic acid, 4-[methyl(trifluoroacetyl)amino]- | HCID 10514620 | — |
| 生成物 | Diisopropylether ethyl acetate | HCID 22281796 | — |
反応手順
4-(N-Methyltrifluoroacetamido)benzoic acid may be prepared in the following manner: a solution of trifluoroacetic anhydride (43.75 g) in anhydrous diethyl ether (50 cc) is added to a solution of 4-methylaminobenzoic acid (21 g) in anhydrous diethyl ether (200 cc) while the temperature is maintained in the vicinity of 0° C. The reaction mixture is then stirred for 20 hours at a temperature in the region of 20° C. and is thereafter concentrated to dryness under reduced pressure (2.7 kPa). On recrystallization of the residue obtained in a diisopropyl ether/ethyl acetate mixture (80:20 by volume), 4-(N-methyltrifluoroacetamido)benzoic acid (7.5 g), m.p. 175° C., is obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04994569 |
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| 出典データセット | uspto-grants-1991_02 |
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| ORD ID | ord-a22dcb7959d248adbede47b43d95ab2f |
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| 出典メモ | uspto-grants-1991_02 |
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