反应详情

Degassed toluene (0.10 mL) was added to t-butyl-(1-{2-[4-(1-ethyl-1-{4-[4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl]-3-methyl-phenyl}-propyl)-2-methyl-phenyl]-ethyl}-2,2-dimethyl-propoxy)dimethylsilane (Example 24-(1); 25.2 mg, 0.0415 mmol), palladium (II) acetate (1.6 mg, 0.071 mmol), 2-dicyclohexylphosphino-2′,6′-dimethoxy-1,1′-biphenyl (6.0 mg, 0.015 mmol) and potassium phosphate (24.5 mg, 0.115 mmol), and the mixture was stirred in a nitrogen atmosphere for three minutes. Then, a solution of (S)-t-butoxycarbonylamino-(4-chloro-phenyl)acetic acid methyl ester (Example 166-(1); 17.9 mg, 0.0597 mmol) in toluene (0.10 mL) and water (20 μL) were added, and the mixture was heated while stirring at an external temperature of 95 to 104° C. for one hour. The reaction mixture was diluted with diethyl ether and filtered through cotton plug, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel chromatography (hexane/ethyl acetate=10/1) to give the title compound (20.8 mg, 67%).

1. customDegassed toluene (0.10 mL)
2. temperaturethe mixture was heated
3. stirringwhile stirring at an external temperature of 95 to 104° C. for one hour
4. filtrationfiltered through cotton plug
5. concentrationthe filtrate was concentrated under reduced pressure
6. customThe residue was purified by silica gel chromatography (hexane/ethyl acetate=10/1)