化工社化工社 化学情報印刷レポート · 研究参考用
Nitromethane → Methyl 3-methyl-4-nitrobutanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Nitromethane | HCID 6375 | — |
| 反応物 | 1,1,3,3-Tetramethylguanidine | HCID 66460 | — |
| 反応物 | Methyl Crotonate | HCID 638132 | — |
| 溶媒 | Ethyl Acetoacetate | HCID 8868 | — |
| 生成物 | Methyl 3-methyl-4-nitrobutanoate | HCID 13633418 | 100% |
反応手順
3 g (29.9 mmol) of trans-2-butenoic acid methyl ester and 0.69 g (5.99 mmol) of tetramethylguanidine and 9.14 g (149 mmol) of nitromethane were mixed. The resulting mixture was stirred at room temperature for 24 days. 100 mL of ethylacetoacetate was added to the solution and the reaction solution was washed with water, then an organic layer was dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, then the residue was purified by column chromatography to give 5.7 g (23.6 mmol) of the title compound in a yield of 100%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07879848B2 |
| 出典データセット | uspto-grants-2011_02 |
| ORD ID | ord-13469d9491184703a32c02a51d91c222 |
| 出典メモ | uspto-grants-2011_02 |