反应详情

To a solution of the compound (2 g) prepared in Example 32 in tetrahydrofuran (35 mL), 1-methyl-2-pyrrolidone (5.2 mL), tris(2,4-pentanedionato)iron(III) (413.5 mg), and isobutyl magnesium bromide (2M diethyl ether solution, 4.68 mL) were added thereto, followed by stirring at room temperature for 4 hours. The reaction mixture was added with a saturated aqueous ammonium chloride solution and the mixture was extracted with t-butyl methyl ether. The organic layer was successively washed with a saturated aqueous ammonium chloride solution, water, and brine, dried and concentrated. Thus, the obtained residue was purified by silica gel column chromatography (hexane:tetrahydrofuran=50:1 to 20:1) to thereby give the title compound (922.5 mg) having the following physical properties.

1. extractionthe mixture was extracted with t-butyl methyl ether
2. washThe organic layer was successively washed with a saturated aqueous ammonium chloride solution, water, and brine
3. customdried
4. concentrationconcentrated
5. customThus, the obtained residue was purified by silica gel column chromatography (hexane:tetrahydrofuran=50:1 to 20:1)