2,4-Dichloro-6-fluorobenzonitrile

反応条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 2,4-dichloro-6-fluorobenzonitrile (3.87 mmol) in 15 mL THF was added a solution of BH3 (15.5 mmol, 1M in THF) and the mixture was stirred at 60° C. for 1 h. After cooling to 0° C., water was added followed by MeOH and the mixture was then heated to 70° C. for 10 min. The solvent was evaporated, the residue was taken up in water and EtOAc. The aqueous phase was separated, basified with 1M NaOH and it was extracted 3 times with EtOAc. The combined organic layers were dried over MgSO4 and concentrated in vacuo to obtain the desired product as yellow oil. After cooling to 0° C. the mixture was then heated to 70° C. for 10 min The solvent was evaporated The aqueous phase was separated was extracted 3 times with EtOAc The combined organic layers were dried over MgSO4 concentrated in vacuo

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 2,4-dichloro-6-fluorobenzamide (5.07 mmol) (US 20060178386) in 74 mL DCM were added Et3N (15.2 mmol) followed by TFAA (10.1 mmol) at 0° C. After 30 min, water was added, the organic layer was separated and concentrated in vacuo. Purification with CC (KP-SIL™ from Biotage) using Hept/EtOAc ( 4/1 to ⅓) gives the desired compound as colorless solid. the organic layer was separated concentrated in vacuo Purification with CC (KP-SIL™ from Biotage)