関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | tert-Butyl methyl malonate | HCID 2733872 | — |
| 反応物 | 5-Chloro-N,N-dimethyl-2-nitrobenzamide | HCID 22934807 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 68760855 | HCID 68760855 | 80.5% |
反応手順
Sodium hydride (350 mg) was dissolved in dimethylformamide (10 mL)), and the solution was cooled to 0° C. After addition of tert-butyl methyl malonate (1.52 g), the mixture was stirred for one hour, and the 5-chloro-N,N-dimethyl-2-nitrobenzamide (1.0 g) obtained in Example 2a) was added thereto. The mixture was stirred at 70° C. for 4.5 hours and water was added thereto. The resulting solution was concentrated, diluted with ethyl acetate and washed with water. The organic layer was dried over sodium sulfate and purified by column chromatography on silica gel with ethyl acetate:hexane=1:1 to give the title compound (1.29 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07538140B2 |
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| 出典データセット | uspto-grants-2009_05 |
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| ORD ID | ord-e35f076fe60b47d98db6c6cc01f6b664 |
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| 出典メモ | uspto-grants-2009_05 |
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