Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium Chloride → Pyridine-3-sulfonyl chloride
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium Chloride | HCID 5234 | — |
| 반응물 | Phosphorus oxychloride | HCID 24813 | — |
| 반응물 | Phosphorus pentachloride | HCID 24819 | — |
| 반응물 | 3-Pyridinesulfonic acid | HCID 69468 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 용매 | tert-Butyl methyl ether | HCID 15413 | — |
| 생성물 | Pyridine-3-sulfonyl chloride | HCID 3164136 | 94.3% |
반응 단계
A mixture of pyridine-3-sulfonic acid (10.3 g, 64.8 mmol), phosphorus pentachloride (20.82 g, 100 mmol) and phosphorus oxychloride (10 mL, 109 mmol) was heated to reflux for 3 h (according to J. Org. Chem. 1989, 54(2), 389.). Evaporated to dryness to give a yellow solid, dissolved in ice water and methyl-tert-butyl ether, added cautiously sat. NaHCO3-sol. until neutralized, saturated with solid NaCl, separated phases, dried organic layer over Na2SO4. Removal of the solvent in vacuum to give the title compound as an orange liquid (10.85 g, 94%). MS (ISP) 178.1 [(M+H)+] and 180.0 [(M+2+H)+].
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07446113B2 |
| 출처 데이터셋 | uspto-grants-2008_11 |
| ORD ID | ord-f04bdb6b900a43cb9eb113fee6b6c913 |
| 출처 메모 | uspto-grants-2008_11 |