反应详情

温度

0 °C

A solution of KHMDS (0.9 mL, 3.20 equiv) in toluene (0.5M) was added dropwise to a stirred solution of Ph3PCH3I (180 mg, 3.02 equiv) in tetrahydrofuran (3 mL) at 0° C. and the resulting mixture was stirred at 0° C. for 30 min. To this was added a solution of 9-fluoro-10-(3-(5-formylisoxazole-3-yl)-3-hydroxybut-1-yn-1-yl)-5,6-dihydrobenzo[f]imidazo[1,2-d][1,4]oxazepine-2-carboxamide (60 mg, 0.15 mmol, 1.00 equiv) in tetrahydrofuran (0.2 mL) dropwise at 0° C. The resulting solution was stirred for 3 h at room temperature. The crude product was purified by Prep-HPLC with the following conditions (1#-Pre-HPLC-006(Waters)): Column, SunFire Prep C18 OBD Column, 5 um, 19*150 mm; mobile phase, Water with 10 mmol NH4HCO3 and CH3CN (25% CH3CN up to 40% in 10 min, up to 95% in 2 min, down to 25% in 2 min); Detector, UV 254/220 nm giving the titled compound (10%) as a light yellow solid.

1. stirringThe resulting solution was stirred for 3 h at room temperature
2. customThe crude product was purified by Prep-HPLC with the following conditions (1#-Pre-HPLC-006(Waters))
3. waitup to 95% in 2 min
4. waitdown to 25% in 2 min)