반응식
[Cl:1][C:2]1[N:7]=[C:6]([C:8]([O:10][CH3:11])=[O:9])[CH:5]=[C:4](Cl)[N:3]=1.C([Sn](CCCC)(CCCC)[C:18]([O:20][CH2:21][CH3:22])=[CH2:19])CCC.[F-].[K+].CC(OC)(C)C>CN(C=O)C.O.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[Cl:1][C:2]1[N:7]=[C:6]([C:8]([O:10][CH3:11])=[O:9])[CH:5]=[C:4]([C:18]([O:20][CH2:21][CH3:22])=[CH2:19])[N:3]=1참가 물질
8
반응물 4
생성물 1
시약·촉매·용매 3
반응 조건
- 온도
- 94 °C
실험 절차
Methyl 2,6-dichloropyrimidine-4-carboxylate (8.44 g, 40.77 mmol) and bis(triphenylphosphine)-palladium(II) chloride (0.572 g, 0.82 mmol) in DMF (80 mL) was degased. Tributyl(1-ethoxy-vinyl)tin (14.46 mL, 42.81 mmol) was added under argon. The mixture was heated at 94° C. for 1 h. The mixture was poured into a solution of potassium fluoride (30 g) in water (400 mL). MTBE (300 mL) was added and the mixture was stirred for 10 min. The mixture was filtered and the filter was washed with 200 mL of MTBE. The filtrate was washed with brine (100 mL), dried over sodium sulfate and the solvents were evaporated. The residue purified by column chromatography on silica eluting with DCM to give the title compound as a solid (7.40 g, 75%).
후처리
- filtrationThe mixture was filtered
- washthe filter was washed with 200 mL of MTBE
- washThe filtrate was washed with brine (100 mL)
- dry with materialdried over sodium sulfate
- customthe solvents were evaporated
- customThe residue purified by column chromatography on silica eluting with DCM
출처 및 근거
- ORD 기록
- ord-04fc7098ba644efc9570b0c89b16e660
- 출처 데이터셋
- uspto-grants-2016_09
- 특허 번호
- US09439904B2
연결된 노트
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