関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1,4-Difluoro-2-methyl-5-nitrobenzene | HCID 230658 | — |
| 反応物 | Benzyl 2-cyanoacetate | HCID 560818 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Benzyl 2-cyano-2-(4-fluoro-5-methyl-2-nitrophenyl)acetate | HCID 58437495 | 81.4% |
反応手順
A suspension of 1,4-difluoro-2-methyl-5-nitrobenzene (1.00 g), cyanoacetic acid benzyl ester (1.01 g) and potassium carbonate (1.76 g) in N,N-dimethylformamide (20.0 mL) was stirred at 60° C. for 1 day. To this reaction mixture was added 1 mol/L hydrochloric acid (25.4 mL), and this mixture was extracted with diethyl ether. This organic layer was washed with brine, and dried over anhydrous magnesium sulfate, and filtered. The solvent was removed under reduced pressure. This residue was washed with ethanol to give the title compound (1.54 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08993616B2 |
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| 出典データセット | uspto-grants-2015_03 |
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| ORD ID | ord-0e84a413efe6400cac12a9b7e5204e6a |
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| 出典メモ | uspto-grants-2015_03 |
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