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Butanoic acid, 4-chloro-4-oxo-, ethyl ester → Ethyl 4-[(4-nitrobenzyl)amino]-4-oxobutanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Butanoic acid, 4-chloro-4-oxo-, ethyl ester | HCID 84648 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 4-Nitrobenzylamine hydrochloride | HCID 11252467 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Ethyl 4-[(4-nitrobenzyl)amino]-4-oxobutanoate | HCID 47312066 | 87% |
反応手順
A mixture of 4-nitrobenzylamine hydrochloride (8.0 g), ethyl 4-chloro-4-oxobutanoate (10.47 g), saturated aqueous sodium hydrogen carbonate (100 ml) and ethyl acetate (100 ml) was stirred at room temperature for 2 hrs. The reaction mixture was extracted with ethyl acetate. The organic layer was washed with water, dried over anhydrous magnesium sulfate, and concentrated. Recrystallization of the residue from ethyl acetate-hexane gave ethyl 4-[(4-nitrobenzyl)amino]-4-oxobutanoate (10.3 g, 87%) as colorless prism crystals. melting point: 104-106° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07423159B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-43ba75e21b7741b1b86881fd744ec663 |
| 出典メモ | uspto-grants-2008_09 |