反应详情

Dimethyl [1-(methylidyneimino)-2-oxopropyl]phosphonate (27.9 mg, 0.15 mmol, 1.00 equiv) in methanol (0.2 mL) was added dropwise to a stirred mixture of 9-fluoro-10-(3-(5-formylisoxazol-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) and potassium carbonate (39 mg, 0.28 mmol, 2.00 equiv) in methanol (1.5 mL) at room temperature. The resulting mixture was stirred for 12 h at room temperature and the solids were filtered out. The crude product (50 mg) 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 mmolNH4HCO3 and CH3CN (22% CH3CN up to 43% in 15 min, up to 95% in 2 min, down to 22% in 2 min); Detector, UV 254/220 nm to give 12.7 mg of the titled compound (21%) as a colorless solid.

1. filtrationthe solids were filtered out
2. customThe crude product (50 mg) was purified by Prep-HPLC with the following conditions (1#-Pre-HPLC-006(Waters))
3. waitColumn, SunFire Prep C18 OBD Column, 5 um, 19*150 mm, mobile phase, Water with 10 mmolNH4HCO3 and CH3CN (22% CH3CN up to 43% in 15 min
4. waitup to 95% in 2 min
5. waitdown to 22% in 2 min)