Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium hydride → N-(5-nitro-2-(pyrrol-1-yl)phenylmethyl)iminodicarboxylic acid di-tert-butyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Di-tert-butyl Iminodicarboxylate | HCID 279800 | — |
| 반응물 | 5-Nitro-2-(pyrrol-1-yl)benzyl bromide | HCID 18474002 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | N-(5-nitro-2-(pyrrol-1-yl)phenylmethyl)iminodicarboxylic acid di-tert-butyl ester | HCID 54574337 | 74% |
반응 단계
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%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06414005B1 |
| 출처 데이터셋 | uspto-grants-2002_07 |
| ORD ID | ord-19e89b8f35bd47a78da4095de7164f59 |
| 출처 메모 | uspto-grants-2002_07 |