反应详情

To a solution of (4-(5-amino-3-tert-butyl-1H-pyrazol-1-yl)phenyl)methanol (Ito, K. et al., WO 2010/067131) (8.50 g, 35.0 mmol) and 1H-imidazole (2.71 g, 39.8 mmol) in dry THF (100 mL) under N2 was added chlorotriisopropylsilane (8.16 mL, 38.1 mmol) and the reaction mixture maintained at RT for 5 days. The resulting mixture was evaporated in vacuo and the residue was partitioned between EtOAc (250 mL) and water (100 mL). The organic layer was separated and was washed with (water (100 mL) and brine (80 mL) and then dried and evaporated in vacuo to afford the title compound, Intermediate A12 as a dark red solid (14.6 g, 97%); Rt 3.26 min (Method 2); m/z 402 (M+H)+, (ES+).

1. customThe resulting mixture was evaporated in vacuo
2. customthe residue was partitioned between EtOAc (250 mL) and water (100 mL)
3. customThe organic layer was separated
4. washwas washed with (water (100 mL) and brine (80 mL)
5. customdried
6. customevaporated in vacuo