Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Cesium carbonate → 2-chloro-N-(2,4-dichloro-5-methoxyphenyl)-5-methylpyrimidin-4-amine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 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 | — |
| 반응물 | 1-Bromo-2,4-dichloro-5-methoxybenzene | HCID 19607721 | — |
| 촉매 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 2-chloro-N-(2,4-dichloro-5-methoxyphenyl)-5-methylpyrimidin-4-amine | HCID 57516481 | — |
반응 단계
To a solution of 2-chloro-5-methylpyrimidin-4-amine (44.8 mg, 0.31 mmol) in 1,4-dioxane (20 mL) was added 1-bromo-2,4-dichloro-5-methoxybenzene (96 mg, 0.37 mmol), Cs2CO3 (408 mg, 1.25 mmol), Pd2(dba)3 (37 mg, 0.04 mmol), and 4,5-bis(diphenylphosphino)-9,9-dimethyxanthene (Xant Phos, 70 mg, 0.12 mmol). The mixture was heated under reflux for 4 h under Ar. The solid was filtered off and the filtrate washed with brine (1×100 mL). The organic solution was separated and dried (Na2SO4). The solvent was removed in vacuo. The crude product was used for next reaction without purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08138199B2 |
| 출처 데이터셋 | uspto-grants-2012_03 |
| ORD ID | ord-c3f8cc4f336b426893ca41899a6ba0d9 |
| 출처 메모 | uspto-grants-2012_03 |