indium(III)chloride → HCID 58392362, compound

Participants

Reaction Steps

2.05 g (9.27 mmol) of indium(III) chloride were added to 2.50 g (8.50 mmol) of the compound from Example 192A and 1.62 g (7.72 mmol) of the compound from Example 86A in 31 ml of 1,2-dichloroethane under argon and reflux, and the mixture was heated under reflux for 2.5 h. A further 2.00 g (9.04 mmol) of indium(III) chloride were added, and the mixture was heated under reflux for a further 2 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 1/1) and by preparative HPLC (RP18 column; mobile phase: acetonitrile/water gradient) to result in 13.0 mg (0.3% of theory) of the title compound as mixture of diastereomers.

Provenance & Evidence