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
12/01 2009 15:21:58 +0100 To ethyl 7-bromobenzofuran-2-carboxylate (0.900 g, 3.34 mmol) and 1-(2-(pyridin-2-yl)ethyl)piperazine (0.672 g, 3.51 mmol) in dry degassed dioxane (13 mL) were added Cesium carbonate (1.417 g, 4.35 mmol), 2-Dicyclohexylphosphino-2',4',6'-triisopropylbiphenyl (0.159 g, 0.33 mmol) and Tris(dibenzylideneacetone)dipalladium(0) (0.153 g, 0.17 mmol) under argon and the reaction heated at 95°C o/n. All starting material consumed. Water and DCM were added and the layers separated. The aq phase was extracted with DCM (3x). The combined org phases were washed with water, dried (MgSO4), filtered and evaporated. The crude was purified by flash chrom. (SiO2; DCM/MeOH 95/5) to give EN02198-25-001: 47.3 mg (fraction 12 from the flash) of the product as a pale yellow solid. This batch was submitted to test. EN02198-25-002: 0.460 g (fractions 11 and 13-18 from the flash) of the product as a pale brown solid.
출처 및 근거
- ORD 기록
- ord-61dd76cabf5f48cb8028fe718c7f9d72
- 출처 데이터셋
- 750 AstraZeneca ELN dataset
- 원본 링크
- 출처 보기
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