HCID 58370136、化合物 → HCID 68840871、化合物
反応式
[CH3:1][O:2][C:3](=[O:21])[C:4]([NH:7][C:8]([C:10]1[CH:19]=[CH:18][C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[C:11]=1Br)=[O:9])([CH3:6])[CH3:5]>C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.Cl[Pd]Cl>[CH3:1][O:2][C:3](=[O:21])[C:4]([CH3:6])([NH:7][C:8]([C:10]1[CH:19]=[CH:18][C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[C:11]=1[C:16]#[C:15][CH2:14][CH2:13][C:12]1[CH:17]=[CH:18][CH:19]=[CH:10][CH:11]=1)=[O:9])[CH3:5]参加物
3
反応条件
- 温度
- 130 °C
実験手順
40 mg 2-[(1-bromo-naphthalene-2-carbonyl)-amino]-2-methyl-propionic acid methyl ester and 0.8 mg bis(triphenylphosphine)palladium(II)chloride were placed in a reaction vial, which was evaporated and backfilled with argon three times. Via septum 18 mg of 4-phenyl-1-butyne, 180 μl diethylamine and 0.2 ml abs. DMF were added. In a microwave reactor the reaction was heated to 130° C. for 5 min. Then, water and ethyl acetate were added, the layers were separated, and the aqueous phase was extracted with ethyl acetate twice. The combined organic layers were dried over magnesium sulphate and concentrated. The resulting residue was purified by chromatography on silica (ethyl acetate/heptane) to yield 25 mg of 2-methyl-2-{[1-(4-phenyl-but-1-ynyl)-naphthalene-2-carbonyl]-amino}-propionic acid methyl ester.