関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Propanenitrile, 3-(methylamino)- | HCID 69656 | — |
| 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-methyl-N-beta-cyanoethylamino)quinoline | HCID 18994609 | 100.1% |
反応手順
19.08 g of sodium carbonate are added to a solution of 16.3 g of 2-chloro-3-ethoxycarbonyl-6,7-difluoroquinoline and 10 g of N-methyl-N-(β-cyanoethyl)amine in 160 cm3 of toluene. The suspension obtained is heated to reflux 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 50 cm3 of water. The organic phase is concentrated to dryness under reduced pressure (20 kPa) at approximately 50° C. 19.17 g of 3-ethoxycarbonyl-6,7-difluoro-2-[N-methyl-N-(β-cyanoethyl)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 |
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| 特許番号 | US05484921 |
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| 出典データセット | uspto-grants-1996_01 |
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| ORD ID | ord-ab5d2b91634741eab3d51539c14eb519 |
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| 出典メモ | uspto-grants-1996_01 |
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