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Toluene → N-Cyanoacetylethylcarbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Carbamic acid, ethyl ester | HCID 5641 | — |
| 反応物 | Cyanoacetic acid | HCID 9740 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N-Cyanoacetylethylcarbamate | HCID 23112 | 67% |
反応手順
2-cyanoacetic acid (85 g, 1 mol) and ethyl aminoformate (89 g, 1 mol) were added to toluene (500 mL). To the mixture was slowly added phosphorus oxychloride (45 mL, 0.5 mol), and then added DMF (5 mL). The reaction was conducted at 70° C. for 2 h. After cooling, water (500 mL) was added to the reaction solution to quench phosphorus oxychloride. The reaction is filtered by suction. The filtered cake was washed with ethyl ether and dried to produce a white solid (104 g) in a yield of 67%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08822465B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-710c1d615b944b7f9adc6d68cc7a8ce0 |
| 出典メモ | uspto-grants-2014_09 |