反应详情

温度

80 °C

To a mixture of 2-bromo-1-(4-(5-(5-phenyl-4-propylisoxazol-3-yl)-1,2,4-oxadiazol-3-yl)phenyl)ethanol (30 mg, 0.066 mmol) and tert-butyl azetidine-3-carboxylate, AcOH (21.52 mg, 0.099 mmol) in DMSO (2 mL) was added TEA (0.028 mL, 0.198 mmol). The reaction mixture was heated at 80° C. for 2 hours. The reaction mixture was filtered and purified by HPLC. HPLC conditions: PHENOMENEX® Luna C18 5 micron column (250×30mm); 30-100% CH3CN/water (0.1% TFA); 25 minute gradient; 30 mL/min. Isolated fractions were obtained with the correct mass were freeze-dried overnight to yield 10 mg of Preparation 1D. MS (m+1)=531. HPLC Peak RT=3.67 minutes (Analytical Method A). Purity=92%.

1. filtrationThe reaction mixture was filtered
2. custompurified by HPLC
3. custom25 minute
4. customIsolated fractions were obtained with the correct mass
5. customwere freeze-dried overnight
6. customto yield