참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Acetate | HCID 517044 | — |
| 반응물 | Isopropyl 4-bromobenzoate | HCID 603913 | — |
| 반응물 | Di-tert-butyl[3,4,5,6-tetramethyl-2',4',6'-tris(propan-2-yl)-[1,1'-biphenyl]-2-yl]phosphane | HCID 11953610 | — |
| 반응물 | HCID 178513763 | HCID 178513763 | — |
| 촉매 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 용매 | Isopropanol | HCID 3776 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | HCID 178459390 | HCID 178459390 | — |
반응 단계
A round-bottomed flask was charged with 2-propanol (595 mL), and nitrogen was bubbled through the 2-propanol for 2 hours. Pd2(dba)3 (1.63 g, 1.78 mmol) and di-tert-butyl(2′,4′,6′-triisopropyl-3,4,5,6-tetramethylbiphenyl-2-yl)phosphine (3.43 g, 7.14 mmol) were added, and the mixture was stirred for 20 minutes. Potassium acetate (17.5 g, 178 mmol), 3-amino-1H-pyrazole-4-carboxamide (15.0 g, 119 mmol), and isopropyl 4-bromobenzoate (34.7 g, 143 mmol) were then added, and the reaction mixture was heated to 75° C. for 6.5 hours. The reaction mixture was then cooled to 23° C., diluted with EtOAc (500 mL), and filtered through celite. The filtrate was adsorbed onto silica gel in vacuo and purified by MPLC on silica gel (using a gradient elution of 30-90%, EtOAc/hexanes) to afford the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US09328099B2 |
|---|
| 출처 데이터셋 | uspto-grants-2016_05 |
|---|
| ORD ID | ord-d31c3e5b25124af080468c855828aabe |
|---|
| 출처 메모 | uspto-grants-2016_05 |
|---|
