化工社化工社 化学情報印刷レポート · 研究参考用
Nitromethane → Ethyl 3-(4-chlorophenyl)-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 | 2-Propenoic acid, 3-(4-chlorophenyl)-, ethyl ester | HCID 201471 | — |
| 生成物 | Ethyl 3-(4-chlorophenyl)-4-nitrobutanoate | HCID 11097654 | 92.9% |
反応手順
The solution of ethyl 4-chlorocinnamate (12.6 g) and N,N,N′,N′-tetramethylguanidine (1.2 g) in nitromethane (36.6 g) was kept at rt for three days. The excess of nitromethane was evaporated and the residue dissolved in diethyl ether (250 ml). The organic layer was washed with 2M HCl (2×150 ml), dried (sodium sulfate), and evaporated. The residue was subjected to purification by flash chromatography on silica gel (petrol ether/ethyl acetate 10:1) to give ethyl 3-(4-chlorophenyl)-4-nitrobutanoate (15.1 g) as yellowish oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08912186B2 |
| 出典データセット | uspto-grants-2014_12 |
| ORD ID | ord-5c511d6b0d524f17a4214faf2eba502b |
| 出典メモ | uspto-grants-2014_12 |