反应详情

A solution of 200 mg (0.888 mmol) (2E)-2-[(3-methyl-1H-indazol-5-yl)methylidene]-3-oxobutanenitrile (Example 2A), 226 mg (0.888 mmol, approx. 50% purity) 4-hydroxy-5,5-dimethyl-1,5-dihydro-2H-pyrrol-2-one [K. Matsuo et al., Chem. Pharm. Bull. 1984, 32, 3724-3729] and 102 mg (1.332 mmol) ammonium acetate in acetic acid (4 ml) was stirred at 100° C. for 15 min. The reaction mixture was concentrated under reduced pressure, and the residue was purified first by preparative RP-HPLC (acetonitrile/water+0.1% TFA gradient) and then by preparative TLC (eluent: dichloromethane/methanol 10:1) to give 33 mg (11% of th.) of the title compound.

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. customthe residue was purified first by preparative RP-HPLC (acetonitrile/water+0.1% TFA gradient)