Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → 2-Chloro-4-fluoro-5-[(methylamino)sulfonyl]benzoic acid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Methylamine | HCID 6329 | — |
| 반응물 | 2-Chloro-3-chlorosulfonyl-4-fluorobenzoic acid | HCID 86608473 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 2-Chloro-4-fluoro-5-[(methylamino)sulfonyl]benzoic acid | HCID 58728292 | 89% |
반응 단계
20.02 g (73.4 mmol) of 2-chloro-3-chlorosulfonyl-4-fluorobenzoic acid was added as a solid to a cooled solution of 10.5 mL of methylamine (40% aqueous solution, 293.6 mmol) in 400 mL of water. Reaction was monitored by LC/MS and complete after one hour. The reaction was acidified to pH=1 with concentrated HCl, and solid precipitated out. Product was obtained by filtration. 17.54 g obtained as a pale tan solid (89% yield). 1H NMR (300 MHz, DMSO-d6) δ13.83-14.01 (br, 1H), 8.21-8.26 (d, 1H, J=9.11 Hz), 7.98-8.03 (q, 1H, J=4.82), 7.88-7.92 (d, 1H, J=9.11 Hz), 2.55-2.56 (d, 3H, J=4.82 Hz).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07645771B2 |
| 출처 데이터셋 | uspto-grants-2010_01 |
| ORD ID | ord-8a06829d0b7b48edb77db886836d0741 |
| 출처 메모 | uspto-grants-2010_01 |