Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Pyridine → Benzenesulfonamide, 4-chloro-3-nitro-N-phenyl-
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Pyridine | HCID 1049 | — |
| 반응물 | Aniline | HCID 6115 | — |
| 반응물 | 4-Chloro-3-nitrobenzenesulfonamide | HCID 7324 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | Benzenesulfonamide, 4-chloro-3-nitro-N-phenyl- | HCID 67302 | 96.2% |
반응 단계
Two portions of 4-Chloro-3-nitrobenzenesulfonamide (1.73 g, 6.78 mmol) were dissolved in CH2Cl2 (7.0 mL) in reaction flasks. Aniline (757 mg, 8.13 mmol) was added drop-wise at room temperature, followed by slow additions of pyridine (2.0 mL). After 16 h of continued stirring, the reaction mixtures were diluted with ethyl acetate (50 mL) and washed with 1 M HCl (3×50 mL). The organic phases were dried (MgSO4) and evaporated to brown solids, which upon re-crystallization from ethanol/water gave off-white solid of the product 2.04 g (96%): 1H NMR (CDCl3, 400 MHz) δ 8.24 (d, 1H), 7.80 (dd, 1H), 7.61 (d, 1H), 7.30 (t, 2H), 7.20 (t, 1H), 7.09 (d, 2H), 6.79 (bs, 1H); MS (CI) 310.8 (M−H)−; Purity (HPLC, Hichrom 200×4.6 mm I.D.)>98%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07566715B2 |
| 출처 데이터셋 | uspto-grants-2009_07 |
| ORD ID | ord-cde683c2f4e44cf895a311a14fbafc0e |
| 출처 메모 | uspto-grants-2009_07 |