反应详情

温度

90 °C

To a suspension of 1-[4-chloro-6-(methylamino)-1,3,5-triazin-2-yl]-N-{[2-(trifluoromethyl)phenyl]methyl}-4-piperidinecarboxamide (Intermediate 7d, 75 mg, 0.17 mmol, 1.0 equiv), (2-methylphenyl)boronic acid (29 mg, 0.21 mmol, 1.2 equiv), and Na2CO3 (37 mg, 0.35 mmol, 2.0 equiv) in 3:1 CH3CN:H2O was added Pd(PPh3)4 (10 mg, 0.0088 mmol, 0.05 equiv). The reaction mixture was heated at 90° C. for 1 h. The resulting suspension was filtered through an SCX resin (55 □m, 70 A, 2 g/12 mL giga tubes) using MeOH, and the product was recovered by eluting with 2.0 M NH3 in MeOH. The filtrate was concentrated, and the resulting residue was purified using reverse-phase HPLC (XBridge, 10-80% CH3CN/H2O, 0.1% TFA, 12 min) to afford 25 mg (30%) of the title compound. MS (ES+): m/e 485.2 [M+H]+.

1. filtrationThe resulting suspension was filtered through an SCX resin (55 □m, 70 A, 2 g/12 mL giga tubes)
2. customthe product was recovered
3. washby eluting with 2.0 M NH3 in MeOH
4. concentrationThe filtrate was concentrated
5. customthe resulting residue was purified
6. customreverse-phase HPLC (XBridge, 10-80% CH3CN/H2O, 0.1% TFA, 12 min)