反应详情

温度

175 °C

To a microwave tube charged with 4-bromo-5-fluoro-2,3-dihydro-1H-inden-1-one (500 mg, 2.2 mmol) and a stir bar was added Pd2(dba)3 (40.0 mg, 0.044 mmol), S-phos (45 mg, 0.11 mmol), zinc cyanide (333 mg, 2.84 mmol), DMF (15 mL), and Water (0.15 mL). The tube was sealed, and purged three times with nitrogen. The reaction was then heated to 175° C. for 3 minutes in a microwave reactor. TLC showed formation of the desired product, along with a small amount of the dimethylaniline adduct. The crude product mixture was diluted with EtOAc, washed with brine, dried over sodium sulfate, adsorbed onto silica, and purified by MPLC. After removal of solvent, 5-fluoro-1-oxo-2,3-dihydro-1H-indene-4-carbonitrile was collected.

1. customThe tube was sealed
2. custompurged three times with nitrogen
3. additionThe crude product mixture was diluted with EtOAc
4. washwashed with brine
5. dry with materialdried over sodium sulfate
6. custompurified by MPLC
7. customAfter removal of solvent, 5-fluoro-1-oxo-2,3-dihydro-1H-indene-4-carbonitrile
8. customwas collected