Cesium carbonate → HCID 25270134, compound

Participants

Reaction Conditions

Reaction Steps

Under an argon atmosphere 330 mg (1.20 mmol) 7-methoxy-3-piperidin-4-yl-1,3,4,5-tetrahydro-benzo[d][1,3]diazepin-2-one, 350 mg (1.01 mmol) 6-(3-bromo-benzoyl)-3,4-dimethyl-3H-benzoxazol-2-one and 586 mg (1.80 mmol) caesium carbonate were stirred in 10 mL xylene, then combined with 56 mg (0.090 mmol) BINAP and 20 mg (0.089 mmol) palladium(II)acetate and stirred for 48 h at 100° C. The mixture was evaporated down i. vac., the residue was dissolved in DMF/MeOH and purified by preparative HPLC-MS. The fractions containing the product were combined and the acetonitrile was evaporated down. The aqueous residue was made basic with 1N aqueous sodium hydroxide solution, the precipitate formed was suction filtered and washed with water and dried. The product was again purified by preparative HPLC-MS. The fractions containing the product were combined and freeze-dried.

Provenance & Evidence