참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | 1,4-Dioxane | HCID 31275 | — |
| 반응물 | Phenylboronic Acid | HCID 66827 | — |
| 반응물 | 5-Bromo-3-nitropyridine-2-carbonitrile | HCID 2769698 | — |
| 촉매 | HCID 178418807 | HCID 178418807 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 3-Nitro-5-phenylpicolinonitrile | HCID 46314745 | — |
반응 단계
5-bromo-3-nitropicolinonitrile (1 eq) and phenylboronic acid (1.5 eq) was mixed with 15 mL of 1,4-dioxane and 5 mL of 2 M Na2CO3 aqueous solution in a glass pressure tube. The reaction mixture was degassed by anhydrous N2 stream for 5 min followed by the addition of Pd(dppf)Cl2-DCM (0.1 eq). The reaction mixture was stirred at 100° C. for 3 hours. Then the mixture was diluted with 100 mL of ethyl acetate and washed with water, brine, then dried over MgSO4, filtered, and evaporated under reduced pressure to give crude product, which was triturated by DCM, ether, hexanes to give the pure titled compound. LC/MS (m/z): 226.1 (MH+).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08822497B2 |
|---|
| 출처 데이터셋 | uspto-grants-2014_09 |
|---|
| ORD ID | ord-d9bd29a468344207916a81149c67d060 |
|---|
| 출처 메모 | uspto-grants-2014_09 |
|---|
