関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Ethyl N-ethyl-beta-alaninate | HCID 90223 | — |
| 反応物 | 2-Chloro-3-ethoxycarbonyl-6,7-difluoroquinoline | HCID 9795461 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 3-ethoxycarbonyl-6,7-difluoro-2-[N-ethyl N-(beta-ethoxycarbonylethyl)amino]quinoline | HCID 9842837 | 92.8% |
反応手順
7.8 g of sodium carbonate are added to a solution of 10 g of 2-chloro-3-ethoxycarbonyl-6,7-difluoroquinoline, prepared as described in Application Example 1, and 9.7 g of N-ethyl-N-(b-ethoxycarbonylethyl)amine in 120 cm3 of toluene. The suspension obtained is heated to approximately 90° C. and then stirred for 4 hours at this temperature. The reaction mixture is then cooled to approximately 20° C. and thereafter washed with 3 times 100 cm3 of water. The organic phase is concentrated to dryness under reduced pressure (20 kPa) at approximately 50° C. 13 g of 3-ethoxycarbonyl-6,7-difluoro-2-[N-ethyl-N-(b-ethoxycarbonylethyl)amino]quinoline are obtained in the form of an oil, which is used without further purification for the subsequent steps.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05442070 |
|---|
| 出典データセット | uspto-grants-1995_08 |
|---|
| ORD ID | ord-17311acfc39048cdb36fc053b4c64d82 |
|---|
| 出典メモ | uspto-grants-1995_08 |
|---|