Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Bromine → 4'-(Bromomethyl)-N-t-butyl-3'-fluoro-2-biphenylsulfonamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Bromine | HCID 24408 | — |
| 반응물 | 3-Fluoro-4-methyl-2'-(N-t-butylsulfamoyl)biphenyl | HCID 10087424 | — |
| 촉매 | Tungsten | HCID 23964 | — |
| 용매 | Carbon Tetrachloride | HCID 5943 | — |
| 생성물 | 4'-(Bromomethyl)-N-t-butyl-3'-fluoro-2-biphenylsulfonamide | HCID 10046521 | 81.8% |
반응 단계
A solution of 1.08 g (3.36 mmol) of 3-fluoro-4-methyl-2'-(N-t-butylsulfamoyl)biphenyl (from Step A) in 20 mL of CCl4 was stirred at reflux under irradiation from a 100-watt tungsten lamp as a solution of 3.5 mmol of bromine in approximately 13 mL of CCl4 was added dropwise over 1.5 hour. After being stirred at reflux overnight, the solution was cooled and concentrated. The residue was crystallized from EtOAc-hexane to give 1.10 g of the title compound as an off-white solid, mp 138°-140° C. (estimated purity 87%; contained minor unbrominated and dibrominated contaminants by TLC); mass spectrum (FAB) m/e 400, 402 (M+1)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05411980 |
| 출처 데이터셋 | uspto-grants-1995_05 |
| ORD ID | ord-44e3ba39eab54a15a4de1eaa21287227 |
| 출처 메모 | uspto-grants-1995_05 |