反应详情

温度

70 °C

To a mixture of Compound 1A (100 mg, 0.29 mmol) and (R)-1-phenylethanamine (34.9 mg, 0.29 mmol) in 0.6 mL of DMA was added DIEA (37.2 mg, 0.29 mmol). The mixture was stirred at room temperature for 17 h upon which time DIEA (74.4 mg, 0.58 mmol) and tert-butyl piperidine-4-ylcarbamate (86.4 mg, 0.43 mmol) were added. The mixture was heated at 70° C. for 3 h and cooled to room temperature. TFA (2.00 mL, 260 mmol) was added and the mixture was stirred at room temperature for 1 h. The mixture was concentrated in vacuo and the residue was purified by prep HPLC to give Compound 1C in 62% yield. Compound 1C had an analytical HPLC retention time=1.58 min. (YMC S5 ODS column 4.6×50 mm, 10–90% aqueous methanol over 4 minutes containing 0.2% phosphoric acid, 4 ml/min, monitoring at 220 nm) and a LC/MS M++1=351.

1. additionwere added
2. temperaturecooled to room temperature
3. concentrationThe mixture was concentrated in vacuo
4. customthe residue was purified by prep HPLC