Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
4-Chloro-3-nitrobenzenesulfonamide → 4-(4-Methylpiperazin-1-ylamino)-3-nitrobenzenesulfonamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 4-Chloro-3-nitrobenzenesulfonamide | HCID 7324 | — |
| 반응물 | N,N,N',N'-Tetramethylethylenediamine | HCID 8037 | — |
| 반응물 | 4-Methylpiperazin-1-ylamine dihydrochloride hydrate | HCID 198221 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 4-(4-Methylpiperazin-1-ylamino)-3-nitrobenzenesulfonamide | HCID 4737741 | — |
반응 단계
A 50 mL round-bottomed flask was charged with 4-chloro-3-nitrobenzenesulfonamide (1 g, 4.23 mmol), 4-methylpiperazin-1-amine dihydrochloride (1 g, 5.32 mmol), and N1,N1,N2,N2-tetramethylethane-1,2-diamine (3 mL, 20.01 mmol) in dioxane (10 mL). The reaction mixture was refluxed for 12 hours. After this time, the reaction mixture was cooled to room temperature, the salt filtered off via a Buchner funnel, and the solvent removed in vacuo. The crude product was added to a silica gel column (Analogix, SF65-200g) and purified by eluting with 0-5% methanol in dichloromethane.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09174982B2 |
| 출처 데이터셋 | uspto-grants-2015_11 |
| ORD ID | ord-825071fa8f3242048a042563b5ed0413 |
| 출처 메모 | uspto-grants-2015_11 |