반응식
CCOC(=O)c1cc2cccc(Br)c2o1.c1ccc(CCN2CCNCC2)nc1>C1COCCO1.CC(C)c1cc(C(C)C)c(-c2ccccc2P(C2CCCCC2)C2CCCCC2)c(C(C)C)c1.O=C(/C=C/c1ccccc1)/C=C/c1ccccc1.O=C(/C=C/c1ccccc1)/C=C/c1ccccc1.O=C(/C=C/c1ccccc1)/C=C/c1ccccc1.O=C([O-])[O-].[Cs+].[Cs+].[Pd].[Pd]>CCOC(=O)c1cc2cccc(N3CCN(CCc4ccccn4)CC3)c2o1참가 물질
반응물 2
생성물 1
시약·촉매·용매 4
반응 조건
- 온도
- 95 °C
실험 절차
27/05 2009 13:35:19 +0200 To dry degassed dioxane (30 mL) were added ethyl 7-bromobenzofuran-2-carboxylate (2.30 g, 8.55 mmol) and 1-(2-(pyridin-2-yl)ethyl)piperazine (1.798 g, 9.40 mmol), Cesium carbonate (3.62 g, 11.11 mmol), 2-Dicyclohexylphosphino-2',4',6'-triisopropylbiphenyl (0.407 g, 0.85 mmol) and Tris(dibenzylideneacetone)dipalladium(0) (0.391 g, 0.43 mmol) under argon and the reaction heated at 95°C for 4h. The reaction mixture was filtered and solvent evaporated. The material was purified by flash (SiO2; DCM/MeOH 97/3) to give 0.620 g, but it was not pure enough (EN02198-94-001). A second flash was performed (SiO2; DCM/MeOH 97/3) to give 0.540 g of the product as a yellow solid (EN02198-94-002). 100% pure according to HPLC. The reaction mixture was combined with the reaction mixture in EN02745-56 and hydrolysed.
출처 및 근거
- ORD 기록
- ord-a6ed7cd19836494cb3c62d6a1e160912
- 출처 데이터셋
- 750 AstraZeneca ELN dataset
- 원본 링크
- 출처 보기
연결된 노트
불러오는 중…