Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
4-Bromo-2-iodoaniline → Benzothiazole, 6-bromo-2-methyl-
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 4-Bromo-2-iodoaniline | HCID 823934 | — |
| 반응물 | Thioacetamide | HCID 2723949 | — |
| 촉매 | Ferrocene-1,1'-bis-(diphenylphosphine) | HCID 635956 | — |
| 촉매 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 용매 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 생성물 | Benzothiazole, 6-bromo-2-methyl- | HCID 138448 | 48.2% |
반응 단계
A solution of 4-bromo-2-iodo-phenylamine (1.5 g, 5.0 mmol), thiacetamide (381 mg, 5.0), cupric oxide (280 mg, 3.5 mmol), dppf (56 mg, 0.10 mmol), Pd2(dba)3 (48 mg, 0.052 mmol) in DME was heated at 60° C. for 1 hour, cooled to room temperature, partitioned between water and ethyl acetate. The organic phase was dried (Na2SO4) and concentrated. The concentrate was purified by flash chromatography on silica gel using 20% hexanes/methylene chloride to give 550 mg (40% yield) of the desired product. MS (ESI(+)) m/e 227.8, 229.8 (M+H)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08273736B2 |
| 출처 데이터셋 | uspto-grants-2012_09 |
| ORD ID | ord-0cc6ea8707364b69bf6d9165d5632780 |
| 출처 메모 | uspto-grants-2012_09 |