反应详情

温度

100 °C

3-(4-((1H-imidazol-4-yl)methyl)piperidine-4-carboxamido)phenyl dimethylcarbamate from step D (10 mg, 0.027 mmol), 4-chloro-5-methyl-7H-pyrrolo[2,3-d]pyrimidine (5 mg, 0.03 mmol), and N,N-diisopropylethylamine (23 μL, 0.135 mmol) were combined in isopropanol (0.5 mL). The resulting mixture was heated at 100° C. in a sealed pressure tube for 24 hours. The reaction mixture was cooled and concentrated under vacuum. The residue was purified by prep HPLC (10-95% MeOH:H2O with 0.1% HCOOH), then treated with AcOH in H2O and lyophilized to give the title compound (5.7 mg, 42%) as the acetate salt.

1. temperatureThe reaction mixture was cooled
2. concentrationconcentrated under vacuum
3. customThe residue was purified by prep HPLC (10-95% MeOH:H2O with 0.1% HCOOH)
4. additiontreated with AcOH in H2O