反应详情

96.9 mg (0.44 mmol) of indium(III) chloride and 0.06 ml (0.72 mmol) of trifluoroacetic acid were added to 113 mg (0.40 mmol) of the compound from Example 87A with a purity of 80% and 100 mg (0.48 mmol) of the compound from Example 162A under argon in 4 ml of dichloromethane, and the mixture was heated under reflux for 1 h. It was diluted with dichloromethane and washed with water and saturated aqueous sodium bicarbonate solution, dried over magnesium sulfate, filtered and concentrated. The residue was purified by preparative HPLC (RP18 column; mobile phase: acetonitrile/water gradient with addition of 0.1% formic acid) to result in 69.0 mg (41% of theory) of the title compound as mixture of diastereomers.

1. temperaturethe mixture was heated
2. temperatureunder reflux for 1 h
3. washwashed with water and saturated aqueous sodium bicarbonate solution
4. dry with materialdried over magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated
7. customThe residue was purified by preparative HPLC (RP18 column; mobile phase: acetonitrile/water gradient with addition of 0.1% formic acid)