Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethylacetamide → Ethyl 6-({2-[(5-nitro(2-pyridyl))amino]ethyl}amino)-4-phenylpyridine-3-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethylacetamide | HCID 31374 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 2-(2-Aminoethylamino)-5-nitropyridine | HCID 122425 | — |
| 반응물 | Ethyl 6-chloro-4-phenylpyridine-3-carboxylate | HCID 22142763 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | Ethyl 6-({2-[(5-nitro(2-pyridyl))amino]ethyl}amino)-4-phenylpyridine-3-carboxylate | HCID 22143004 | 70% |
반응 단계
The crude material above, ethyl 6-chloro-4-phenylpyridine-3-carboxylate (140 mg, 0.56 mmol) was mixed with (2-aminoethyl)(5-nitro(2-pyridyl))amine (408 mg, 2.24 mmol), Hünig's base (390 ul), and DMA (2 ml) for 48 hours at 70-75° C. with stirring under argon. The reaction was followed by TLC and HPLC. When judged complete, the reaction was diluted with EtOAc (100 ml) and washed with sat. aq. NaHCO3 (5×30 ml), brine (30 ml), dried with Na2SO4, filtered, and concentrated under reduced pressure. The yellow solid was purified by column chromatography using 5% MeOH in CH2Cl2 as the eluent. The product was dried overnight in vacuo giving ethyl 6-({2-[(5-nitro(2-pyridyl))amino]ethyl}amino)-4-phenylpyridine-3-carboxylate in 70% yield.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07425557B2 |
| 출처 데이터셋 | uspto-grants-2008_09 |
| ORD ID | ord-7ad28e6003144e34a8b89ccba300464e |
| 출처 메모 | uspto-grants-2008_09 |