反应详情

温度

100 °C

Pd(OAc)2 (3.3 mg) is added to a mixture of (2R,6R,11S)-6,11-dimethyl-8-borono-1,2,5,6-tetrahydro-4H-2,6-methano-benzo[d]azocine-3-carboxylic acid tert-butyl ester (0.30 g), 4-chloro-2-methyl-pyrimidine (93 mg), K3PO4 (0.31 g), and 2-dicyclohexylphosphino-2′,6′-dimethoxy-1,1′-biphenyl (11.5 mg) in n-butanol (2 mL) under argon atmosphere. The resulting mixture is heated to 100° C. and stirred at this temperature overnight. After cooling to room temperature, ethyl acetate is added, the resulting mixture is filtered, and the filtrate is concentrated under reduced pressure. The residue is taken up in CH2Cl2 (3 mL) and treated with F3CCO2H (0.5 mL) for 1 h. Then, the solution is concentrated and the residue is purified by HPLC on reversed phase (MeCN/H2O/NH3) to afford the title compound.

1. temperatureAfter cooling to room temperature
2. filtrationthe resulting mixture is filtered
3. concentrationthe filtrate is concentrated under reduced pressure
4. additiontreated with F3CCO2H (0.5 mL) for 1 h
5. concentrationThen, the solution is concentrated
6. customthe residue is purified by HPLC on reversed phase (MeCN/H2O/NH3)