関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethyl malonate | HCID 7943 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Methyl 2-chloro-3-nitrobenzoate | HCID 10751184 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | Dimethyl 2-methoxycarbonyl-6-nitrophenylmalonate | HCID 54355276 | — |
反応手順
Dimethyl malonate (6.0 mL) was added to an ice-cold suspension of 2.1 g of sodium hydride in 15 mL of DMSO. The reaction mixture was then stirred at 100° C. for 1.0 h and then cooled to room temperature. 2-Chloro-3-methoxycarbonyl-nitrobenzene (2.15 g) was added to the above mixture in one portion and the mixture was heated to 100° C. for 1.5 h. The reaction mixture was then cooled to room temperature and poured into ice water, acidified to pH 5, and extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous sodium sulfate and concentrated to give 3.0 g of the dimethyl 2-methoxycarbonyl-6-nitrophenylmalonate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06855730B2 |
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| 出典データセット | uspto-grants-2005_02 |
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| ORD ID | ord-58a5645a0dc64447b7a771be05418a61 |
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| 出典メモ | uspto-grants-2005_02 |
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