Lithium Hydroxide → HCID 66863432, compound

Participants

Reaction Steps

0.222 g of lithium hydroxide is added, in two parts, to a solution of 2.5 g of 3-({1-[bis(4-chlorophenyl)methyl]azetidin-3-yl}methanesulphonylamino)-5-fluorobenzoic acid ethyl ester in a mixture comprising 34 cm3 of tetrahydrofuran and 9 cm3 of water, stirred under an argon atmosphere. The reaction medium is stirred at a temperature in the region of 20° C. for 24 hours. 100 cm3 of a saturated aqueous solution of sodium hydrogen phosphate are then added so as to bring the pH to 5. The aqueous phase is extracted four times with 200 cm3 of ethyl acetate. The combined organic phases are dried over sodium sulphate, filtered through sintered glass and then concentrated to dryness under reduced pressure, to give a foam which is taken up twice with 150 cm3 of ethyl ether. After concentration under reduced pressure, 2.3 g of 3-({1-[bis(4-chlorophenyl)methyl]azetidin-3-yl}methanesulphonylamino)-5-fluorobenzoic acid are obtained in the form of a white solid.

Provenance & Evidence