関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | Ethyl 6-fluoro-7-(pyrrol-1-yl)-1-amino-4-oxo-1,4-dihydroquinoline-3-carboxylate | HCID 13670072 | — |
| 溶媒 | Formic Acid | HCID 284 | — |
| 生成物 | Ethyl 6-fluoro-7-(pyrrol-1-yl)-1-formylamino-4-oxo-1,4-dihydroquinoline-3-carboxylate | HCID 13670073 | — |
反応手順
A solution of 3.15 g (0.01 mol) of ethyl 6-fluoro-7-(pyrrol-1-yl)-1-amino-4-oxo-1,4-dihydroquinoline-3-carboxylate in 25 ml of formic acid is added dropwise to a mixture of 9.5 ml (0.01 mol) of acetic anhydride and 4 ml (0.01 mol) of formic acid, cooled to 0° C., the addition being carried out so as to maintain room temperature ±5° C. The mixture is kept at room temperature for48 hours and poured into a water/ice mixture, and the precipitate formed is filtered off, washed with water and recrystallized from a dimethylformamide/water mixture (1:1) to give a solid melting at 254°-257° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04727080 |
|---|
| 出典データセット | uspto-grants-1988_02 |
|---|
| ORD ID | ord-8adc3019916d41df93e9978debdaa4cb |
|---|
| 出典メモ | uspto-grants-1988_02 |
|---|