Boron Trichloride → HCID 131721197, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of 17 (from Part D) (2.42 g, 4.54 mmol) in CH2Cl2 (100 ml), at -78° C. under nitrogen atmosphere, 1M solution of BCl3 (50 ml, 49.94 mmol) was added dropwise. The reaction mixture was stirred at -78° C. for 4 h and 1:1 mixture of CH2Cl2 /MeOH (100 ml) was added and the reaction mixture was brought to room temperature and the solvents were evaporated to dryness. The residue was coevaporated with MeOH (50 ml) 5 times. The residue obtained was dissolved in water and washed with CHCl3 (50×2) and CCl4 (50 ml). The water layer was evaporated to give a white solid and which was crystallized from EtOH/ether to give the pure 18 (0.94 g, 79.4%) as white crystals: mp 231° C. dec.

Provenance & Evidence