反应详情

33.0 mg (0.15 mmol) of indium(III) chloride and 0.02 ml (0.22 mmol) of trifluoroacetic acid were added to 30.0 mg (0.12 mmol) of the compound from Example 160A and 41.4 mg (0.15 mmol) of the compound from Example 87A with a purity of 82% under argon in 1 ml of 1,2-dichloroethane, and the mixture was heated under reflux for three days. It was concentrated and the residue was taken up in ethyl acetate, washed with saturated aqueous sodium bicarbonate solution and saturated aqueous sodium chloride solution, dried over sodium 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 12.6 mg (23% of theory) of diastereomer 1 and 13.2 mg (24% of theory) of diastereomer 2 of the title compound.

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