Water → HCID 13588529, compound

Participants

Reaction Steps

10.9 g of triphenylphosphine were added to a solution of 13 g of the product of Step 3 in 250 ml of tetrahydrofuran at approximately -5° C. and the mixture was stirred for 5 hours at room temperature. 8.5 ml of water were added and the mixture was stirred for 24 hours at room temperature. The tetrahydrofuran was evaporated off and the residue was taken up in methylene chloride. The mixture was poured into ice-cold 2N hydrochloric acid, followed by extraction with 2N hydrochloric acid, neutralization with sodium bicarbonate and extraction with methylene chloride. The extract was washed with saline solution, dried and evaporated to dryness to obtain 10 g of the expected product melting at 50° C. after crystallization from isopropyl ether.

Provenance & Evidence