反应详情

温度

180 °C

To a 20 mL microwave vial were added 2-(4-bromo-3-fluoro-phenyl)-morpholine-4-carboxylic acid tert-butyl ester (1.5 g, 4.16 mmol) N-methyl-pyrrolidone (10 ml) and copper(I)-cyanide (559 mg, 6.25 mmol). The vial was capped and heated in a microwave synthesizer (Personal Chemistry Emrys Optimizer) at 180° C. for 30 min. The reaction mixture was poured into tert-butylmethylether (150 ml) and extracted with brine (3×50 mL). The organic layers were dried over MgSO4 and concentrated in vacuo. The crude material was purified by flash chromatography (silica gel, 50 g, 0% to 70% ethyl acetate in heptane) to yield a yellow solid (101 mg, 8%), MS (ISP): 307.2 ([M+H]+).

1. customThe vial was capped
2. extractionextracted with brine (3×50 mL)
3. dry with materialThe organic layers were dried over MgSO4
4. concentrationconcentrated in vacuo
5. customThe crude material was purified by flash chromatography (silica gel, 50 g, 0% to 70% ethyl acetate in heptane)