참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 2-Amino-N-methylbenzamide | HCID 308072 | — |
| 반응물 | 2,5-Dichloro-4-iodopyridine | HCID 53400965 | — |
| 시약 | Cesium carbonate | HCID 10796 | — |
| 촉매 | 1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine) | HCID 636044 | — |
| 촉매 | Palladium (II) acetate | HCID 4144353 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 2-[(2,5-Dichloro-4-pyridinyl)amino]-N-methylbenzamide | HCID 57516891 | 69.36% |
반응 단계
2-amino-N-methylbenzamide (110 mg, 0.73 mmol), 2,5-dichloro-4-iodopyridine (200 mg, 0.73 mmol), diacetoxypalladium (8.20 mg, 0.04 mmol), (9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphine) (42.3 mg, 0.07 mmol) and cesium carbonate (357 mg, 1.10 mmol) suspended in 1,4-dioxane (4 mL) was weighed out in a microwave vial and sealed. argon was let to bubble into the mixture for 5 minutes at rt then the resulting mixture was stirred at 100 °C for 1 hour. The reaction mixture was allowed to cool to room temperature under stirring and diluted with dichloromethane. Insolubles were removed by filtration and the filtrate was concentrated. The residue was triturated in DCM, collected by filtration and dried to afford 2-(2,5-dichloropyridin-4-ylamino)-N-methylbenzamide (150 mg, 69.4 %) as a off- white solid.
출처 및 근거
| 출처 데이터셋 | 750 AstraZeneca ELN dataset |
|---|
| ORD ID | ord-b94a4cbc1fbd4100843834a92096e35b |
|---|
| 출처 메모 | 750 AstraZeneca ELN dataset |
|---|