indium(III)chloride → HCID 44595095, compound

Participants

Reaction Steps

1.64 g (7.39 mmol) of indium(III) chloride were added to 2.00 g (6.78 mmol) of the compound from Example 193A and 1.29 g (6.16 mmol) of the compound from Example 86A in 20 ml of 1,2-dichloroethane under argon and reflux, and the mixture was heated under reflux for 1.5 h. This was followed by addition of ethyl acetate and saturated aqueous sodium bicarbonate solution, separation of the phases, drying of the organic phase and concentration. The residue was purified by column chromatography on silica gel (mobile phase: cyclohexane/ethyl acetate 2/1 and 1/1) and by preparative HPLC (RP18 column; mobile phase: acetonitrile/water gradient) to result in 28.0 mg (1% of theory) of diastereomer 1 and 28.0 mg (1% of theory) of diastereomer 2 of the title compound.

Provenance & Evidence