化工社化工社 化学情報印刷レポート · 研究参考用
Sodium hydride → N-(5-nitro-2-(pyrrol-1-yl)phenylmethyl)iminodicarboxylic acid di-tert-butyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Di-tert-butyl Iminodicarboxylate | HCID 279800 | — |
| 反応物 | 5-Nitro-2-(pyrrol-1-yl)benzyl bromide | HCID 18474002 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N-(5-nitro-2-(pyrrol-1-yl)phenylmethyl)iminodicarboxylic acid di-tert-butyl ester | HCID 54574337 | 74% |
反応手順
To a mixture of sodium hydride (60% content, 21 mg), iminodicarboxylic acid di-tert-butyl ester (117 mg) and dimethylformamide (5 ml), a solution in dimethylformamide (3 ml) of the compound (137 mg) obtained in Example 1c was added dropwise under cooling with ice. The reaction mixture was stirred for 2 hours at room temperature and then concentrated at reduced pressure. Brine was added to the resulting residue and the mixture was extracted with ethyl acetate. The organic layer was dried with anhydrous sodium sulfate and then concentrated at reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent; ethyl acetate:n-hexane=1:9) to give the titled compound (yield, 74%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06414005B1 |
| 出典データセット | uspto-grants-2002_07 |
| ORD ID | ord-19e89b8f35bd47a78da4095de7164f59 |
| 出典メモ | uspto-grants-2002_07 |