反应详情

The title compound was prepared by chiral separation (Preparative chiral HPLC, ChiralPak® AS, 20 μm 50×500 mm, mobile phase: n-heptane/EtOH/MeOH (85:10:5)+0.05% DEA, flow rate 68 mL/min, wavelength: 210 nm) of a racemic mixture of N-(4-(chlorodifluoromethoxy)phenyl)-6-((2,4-dihydroxybutyl)amino)-5-(1H-pyrazol-5-yl)nicotinamide (Example 97), slower eluting isomer (Peak 2, tR=12.52 min). Or alternatively, in an analogous fashion to that described in Example 97 using (S)-benzyl(2,4-dihydroxybutyl)carbamate (Stage 98.1) as chiral starting material. HPLC chiral (Chiralpak® AS-H, eluent: n-heptane/EtOH/MeOH (80:12:8)+0.05% DEA, flow rate:1 mL/min, temperature: RT, DAD 300 nm.): tR=9.31 min.

1. washslower eluting isomer (Peak 2, tR=12.52 min)
2. customHPLC chiral (Chiralpak® AS-H, eluent: n-heptane/EtOH/MeOH (80:12:8)+0.05% DEA, flow rate:1 mL/min, temperature: RT, DAD 300 nm.)