反应详情

A solution of crude 4-[[4-fluoro-3-(4-hydroxypiperidine-1-carbonyl)phenyl]methyl]-2H-phthalazin-1-one (2a) (50 mg, 0.131 mmol) in N,N-dimethylacetamide (1 mL) was treated with sodium hydride (60% in mineral oil; 3.8 mg, 0.157 mmol) and the reaction was left stirring at ambient temperature until effervescence had stopped. 2-fluoro-3-methylpyridine (16 mg, 0.144 mmol) was then added and the reaction mixture sealed into a microwave tube, heated to 170° C. and held at that temperature for 250 seconds before cooling to ambient temperature. The mixture was then purified by preparative HPLC to afford the desired material; m/z (LC-MS, ESI+), RT=4.22 (M+H 473.2)

1. waitthe reaction was left
2. customthe reaction mixture sealed into a microwave tube
3. temperatureheated to 170° C.
4. temperaturebefore cooling to ambient temperature
5. customThe mixture was then purified by preparative HPLC