Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ethylenediamine → 2-[(2-Aminoethyl)amino]-8-(2,6-difluorophenyl)-4-(4-fluoro-2-methylphenyl)pyrido[2,3-d]pyrimidin-7(8H)-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ethylenediamine | HCID 3301 | — |
| 반응물 | 8-(2,6-difluoro-phenyl)-4-(4-fluoro-2-methyl-phenyl)-2-methanesulfonyl-8H-pyrido[2,3-d]pyrimidin-7-one | HCID 59639554 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 용매 | Water ethylacetate | HCID 22728543 | — |
| 생성물 | 2-[(2-Aminoethyl)amino]-8-(2,6-difluorophenyl)-4-(4-fluoro-2-methylphenyl)pyrido[2,3-d]pyrimidin-7(8H)-one | HCID 59639577 | 89.6% |
반응 단계
The title compound of Example 7 [8-(2,6-difluorophenyl)-4-(4-fluoro-2-methylphenyl)-2-methanesulfonyl-8H-pyrido[2,3-d]pyrimidin-7-one] (0.89 g, 0.002 mol) in dry THF, stirring at 23°, under Ar, was treated with ethylenediamine (668 uL, 0.01 mol). The color became bright orange. LC MS showed no starting material after 5 min. Reaction was stripped to dryness; the residue taken up in ethyl acetate-water. The layers were separated and the aqueous phase adjusted to pH 10.5 with 10% NaOH. Aqueous phase was extracted twice with ethyl acetate; combined organic layers were dried (Na2SO4), then evaporated to give 0.762 g (89%) of the title compound as an amber glass. LC MS (m/e)=426 (MH+). Rt=1.52 min.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07423042B2 |
| 출처 데이터셋 | uspto-grants-2008_09 |
| ORD ID | ord-d53afcde56f746e2bc7c9b71ad878cb3 |
| 출처 메모 | uspto-grants-2008_09 |