참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Phosphate, Tribasic | HCID 62657 | — |
| 반응물 | 2-Amino-N-methylbenzamide | HCID 308072 | — |
| 반응물 | Bis[2-(diphenylphosphino)phenyl] ether | HCID 4285986 | — |
| 반응물 | 2,5-Dichloro-4-iodopyridine | HCID 53400965 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 2-[(2,5-Dichloro-4-pyridinyl)amino]-N-methylbenzamide | HCID 57516891 | 56.5% |
반응 단계
A 150-mL sealed tube was charged with 2,5-dichloro-4-iodopyridine (3.5 g, 12.78 mmol), 2-amino-N-methylbenzamide (1.919 g, 12.78 mmol) and tripotassium phosphate (8.14 g, 38.3 mmol) in 1,4-dioxane (100 mL). The reaction mixture was degassed with nitrogen for 10 min. Bis(2-diphenylphosphinophenyl)ether (DPEPhos, 0.688 g, 1.278 mmol) and Pd(OAc)2 (0.115 g, 0.511 mmol) were added and the reaction mixture was heated in a 120° C. oil bath over night. The reaction mixture was filtered through celite, which was washed with dioxane. The solvent was evaporated to dryness and the solid was washed with EtOH (10 mL×3) to give 2.14 g (56%) of product as an off white solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US09446034B2 |
|---|
| 출처 데이터셋 | uspto-grants-2016_09 |
|---|
| ORD ID | ord-63006ffb9bab4ecca372336ff57f1a83 |
|---|
| 출처 메모 | uspto-grants-2016_09 |
|---|
