関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Gamma-Valerolactone | HCID 7921 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | Ethyl 2-[(3,4-dichlorophenyl)amino]pyridine-3-carboxylate | HCID 20141561 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 生成物 | 1-(3,4-dichlorophenyl)-4-hydroxy-3-(2-hydroxypropyl)-1,8-naphthyridin-2(1H)-one | HCID 54717823 | — |
反応手順
A stirred mixture of gamma-valerolactone (40 g.), ethyl 2-(3,4-dichlorophenylamino)-nicotinate (20 g.) and potassium t-butoxide (30 g.) was warmed in an atmosphere of nitrogen to 110° C. and kept there for 5 hr. After cooling somewhat the product was poured into 1000 ml. of 5% KOH solution and was allowed to stir overnight. The basic solution was extracted with ether (2×500 ml.) and the aqueous solution was acidified to pH 5 with conc. HCl. The solid was filtered off, washed with water, dried in air then recrystallized from methanol/charcoal to yield the desired product, m.p. 232°-234° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04680298 |
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| 出典データセット | uspto-grants-1987_07 |
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| ORD ID | ord-84aa49adf598419a8dcad6c5ea7cc6b6 |
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| 出典メモ | uspto-grants-1987_07 |
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