反应详情

The 2-oxo-1-[1-oxo-3-(2-trifluoromethylphenyl)-1,2-dihydroisoquinolin-7-yl]pyrrolidin-3-carboxylic acid ethyl (11 mg, 0.025 mmol) prepared in step B of Example 1-45, sodium borohydride (9.5 mg, 0.25 mmol), and calcium chloride (27.7 mg, 0.25 mmol) were dissolved in methanol (5 ml), and the obtained solution was then stirred at a room temperature for 16 hours. Thereafter, the reaction solution was concentrated, and it was then purified using ODS cartridge 5 g (Mega Bond Elut (registered trademark) C18, manufactured by Varian; water methanol=1:0 to 0:1). The resultant was then preparatively separated by preparative HPLC (column: Combi ODS (φ: 28.0 mm×50 mm) manufactured by Wako; developing solvent: 0.05% trifluoroacetic acid-containing water: 0.05% trifluoroacetic acid-containing acetonitrile=90:10 to 5:95), so as to obtain 7-(3-hydroxymethyl-2-oxopyrrolidin-1-yl)-3-(2-trifluoromethylphenyl)-2H-isoquinolin-1-one (5 mg, 50%) in the form of a white amorphous substance.

1. concentrationThereafter, the reaction solution was concentrated
2. customit was then purified
3. customThe resultant was then preparatively separated by preparative HPLC (column: Combi ODS (φ: 28.0 mm×50 mm) manufactured by Wako; developing solvent: 0.05% trifluoroacetic acid-containing water: 0.05% trifluoroacetic acid-containing acetonitrile=90:10 to 5:95)