참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 2,4-Dimethoxybenzylamine | HCID 597250 | — |
| 반응물 | 2-Cyano-3-fluoropyridine | HCID 7060408 | — |
| 용매 | Dimethylacetamide | HCID 31374 | — |
| 생성물 | 3-(2,4-Dimethoxybenzylamino)picolinonitrile | HCID 22293300 | 73.6% |
반응 단계
2,4-Dimethoxybenzylamine (3.29 g, 19.7 mmol) and triethylamine (1.99 g, 19.7 mmol) were added sequentially to a solution of 2-cyano-3-fluoropyridine (2.0 g, 16.4 mmol) (Sakamoto et. al., Chem. Pharm. Bull., 1985, 33, 565-71) in N,N-dimethylacetamide (29 mL). The reaction was heated at 80° C. for 4 h, quenched with water and extracted with diethyl ether (3×). The combined organic extracts were washed water, saturated brine, dried over magnesium sulfate and concentrated. The crude product was purified by flash chromatography (silica gel, 0-12% ethyl acetate (with 0.1 triethylamine) in dichloromethane gradient elution) to produce the title compound (3.25 g). MS 270.3 (M+1).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07745427B2 |
|---|
| 출처 데이터셋 | uspto-grants-2010_06 |
|---|
| ORD ID | ord-eb10cc9be3b049d8b11cf9434a42020e |
|---|
| 출처 메모 | uspto-grants-2010_06 |
|---|