HCID 86731238, compound → HCID 86731237, compound

Participants

Reaction Steps

A mixture of N-(2,4-bis(benzyloxy)-3-fluorophenyl)-4-(cyclopropylmethoxy)-3-fluorobenzamide (12.3 g), 10% palladium-carbon (containing water (50%), 12.0 g) and THF (80 mL) was stirred at room temperature for 20 min under a hydrogen atmosphere. The catalyst was removed by filtration, and the obtained filtrate was concentrated under reduced pressure, and the solid was washed with diethyl ether. To a solution of the obtained solid, hexachloroethane (14.6 g) and triphenylphosphine (16.2 g) in acetonitrile (50 mL) was added triethylamine (10.3 mL) at 0° C., and the mixture was stirred at room temperature for 15 min, and then with heating at 80° C. for 2 hr. The reaction mixture was filtered, the solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give the title compound (3.96 g).

Provenance & Evidence