Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Cesium carbonate → (4-Chloro-3-methyl-phenyl)-(2-chloro-5-methyl-pyrimidin-4-yl)-amine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 반응물 | 5-Bromo-2-chlorotoluene | HCID 609899 | — |
| 반응물 | 1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine) | HCID 636044 | — |
| 반응물 | 2-Chloro-5-methylpyrimidin-4-amine | HCID 4302175 | — |
| 촉매 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | (4-Chloro-3-methyl-phenyl)-(2-chloro-5-methyl-pyrimidin-4-yl)-amine | HCID 57516501 | 38.2% |
반응 단계
A mixture of 2-chloro-5-methyl-pyrimidin-4-ylamine (0.34 g, 2.34 mmol), 4-bromo-1-chloro-2-methyl-benzene (0.58 g, 2.8mmol), Pd2(dba)3 (0.21 g, 0.23 mmol), Xantphos (0.47 g, 0.47 mmol) and cesium carbonate (2.3 g, 7 mmol) were suspended in dioxane (9 mL) microwaved at 160° C. for 20 min. The reaction mixture was cooled to room temperature and centrifuged down. Solvents were then decanted and evaporated. Resulting residue was purified by Hash chromatography on silica gel to afford title compound as yellow solids (0.24 g, 38%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08133900B2 |
| 출처 데이터셋 | uspto-grants-2012_03 |
| ORD ID | ord-173a5f732f8c4b3c9742af166aec9d53 |
| 출처 메모 | uspto-grants-2012_03 |