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1,3-Diethyl 2-oxopropanedioate → Ethyl 5-chloro-2-oxo-1,2-dihydroquinoxaline-3-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,3-Diethyl 2-oxopropanedioate | HCID 69105 | — |
| 反応物 | (2-Amino-3-chlorophenyl)amine | HCID 3462489 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Ethyl 5-chloro-2-oxo-1,2-dihydroquinoxaline-3-carboxylate | HCID 67531483 | 56.5% |
反応手順
10.5 g (73.6 mmol) of 3-chloro-1,2-phenylenediamine and 12.8 g (73.5 mmol) of diethyl ketomalonate were dissolved in ethanol, and the solution was heated to reflux for 3 hours. While heating to reflux, ethanol was added thereto until precipitated crystals dissolved. The reaction mixture was cooled to room temperature, and then precipitated crystals were separated by filtration. The filter cake was washed with cold ethanol, and then dried, to obtain 10.5 g (yield: 51%) of ethyl 5-chloro-2-oxo-1,2-dihydroquinoxaline-3-carboxylate as pale yellow acicular crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08648075B2 |
| 出典データセット | uspto-grants-2014_02 |
| ORD ID | ord-06d5eda75c2e4224b9590b1360ec3dbe |
| 出典メモ | uspto-grants-2014_02 |