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Homophthalic anhydride → (E)-2-[2-[3-[2-[4-(cyclopropyl)-2-thiazolyl]ethenyl]phenylamino]-2-oxoethyl]benzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Homophthalic anhydride | HCID 12801 | — |
| 反応物 | (E)-3-[2-[4-(cyclopropyl)-2-thiazolyl]ethenyl]benzeneamine | HCID 15136080 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | (E)-2-[2-[3-[2-[4-(cyclopropyl)-2-thiazolyl]ethenyl]phenylamino]-2-oxoethyl]benzoic acid | HCID 20084358 | 88.7% |
反応手順
A solution of 5.0 g of (E)-3-[2-[4-(cyclopropyl)-2-thiazolyl]ethenyl]benzeneamine, 3.35 g of homophthalic anhydride, and 100 ml of toluene was heated to reflux for 0.5 hr. After cooling, the solids that formed were collected by filtration and this material was triturated with ethyl ether to yield 7.4 g of (E)-2-[2-[3-[2-[4-(cyclopropyl)-2-thiazolyl]ethenyl]phenylamino]-2-oxoethyl]benzoic acid. Recrystallization from acetonitrile yielded 5.1 g of material; m.p. 200°-201° C. Anal. Calcd for C23H20N2O3S: C, 68.30; H, 4.98; N, 6.93. Found: C, 67.92; H, 4.97; N, 6.83.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05273986 |
| 出典データセット | uspto-grants-1993_12 |
| ORD ID | ord-6eba70f5198f478a853ddef228d2eb90 |
| 出典メモ | uspto-grants-1993_12 |