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Sodium Carbonate → 4-(4-Chloro-2-fluoro-phenylamino)-5,8-dimethoxy-quinoline-3-carbonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 4-Chloro-2-fluoroaniline | HCID 93898 | — |
| 反応物 | 1-Ethoxyethanol | HCID 10129898 | — |
| 反応物 | 4-Chloro-5,8-dimethoxyquinoline-3-carbonitrile | HCID 22466535 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-(4-Chloro-2-fluoro-phenylamino)-5,8-dimethoxy-quinoline-3-carbonitrile | HCID 22466548 | 78.9% |
反応手順
A mixture of 0.148 g of 4-chloro-5,8-dimethoxy-3-quinolinecarbonitrile, 0.102 g of 4-chloro-2-fluoroaniline, and 5 ml of ethoxyethanol was stirred under nitrogen, at reflux temperature for 30 minutes. The mixture was cooled and added to 50 ml of water. To this mixture was added sodium carbonate to pH 9. The product was collected, washed with water, dried, and washed with 10 ml of hexanes-ethyl acetate (4:1) to give 0.168 g of 4-(4-chloro-2-fluoro-phenylamino)-5,8-dimethoxy-quinoline-3-carbonitrile as a solid, mp 197-199° C.; mass spectrum (EI, m/e): M 329.7609.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06002008 |
| 出典データセット | uspto-grants-1999_12 |
| ORD ID | ord-758236d5949d4e47a49938aff0e7d195 |
| 出典メモ | uspto-grants-1999_12 |