Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium hydride → 3-[1-(6-Chloromethyl-pyridin-2-ylmethyl)-indol-3-yl]-4-(1-methyl-indol-3yl)-furan-2,5-dione
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 2,6-Bis(chloromethyl)pyridine | HCID 316654 | — |
| 반응물 | 3-(1-Methyl-indol-3-yl)-4-(indol-3-yl)-furan-2,5-dione | HCID 14855714 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 3-[1-(6-Chloromethyl-pyridin-2-ylmethyl)-indol-3-yl]-4-(1-methyl-indol-3yl)-furan-2,5-dione | HCID 22123282 | — |
반응 단계
Sodium hydride (60% dispersion in oil, 42 mg, 1.8 mmol), 3-(1-methyl-indol-3-yl)-4-(indol-3yl)-furan-2,5-dione (236 mg, 0.7 mmol) and dimethylformamide (8 mL) were stirred at room temperature for 1 h. The reaction mixture was cooled with ice and 2,6-bis-chloromethyl-pyridine (520 mg, 3.0 mmol) was added in one portion. Stirring was continued at room temperature for 65 h. The solvent was evaporated and the residue partitioned between ethyl acetate and water. The organic phase was washed with water, dried with MgSO4, filtered and evaporated. Chromatography (ethyl acetate/heptane:50/50) gave the title compound, which was not pure. Further purification by Kugelrohr distillation (oil pump, 150° C.) afforded 156 mg of the sub-title product.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06153641 |
| 출처 데이터셋 | uspto-grants-2000_11 |
| ORD ID | ord-ba4fd500a14940a49b7e82ea7599e65e |
| 출처 메모 | uspto-grants-2000_11 |