反应详情

2-[(4-Aminobenzyl)methoxyphosphinoylmethyl]-4-methylpentanoic acid benzyl ester (prepared as described in Example 2/Step A) (242 mg, 0.60 mmole) and phthalic anhydride (133 mg, 0.90 mmole) in acetic acid (10 ml) were refluxed for 1 hour. The cooled reaction mixture was concentrated and the residue dissolved in ethyl acetate (100 ml). This solution was washed with saturated sodium bicarbonate solution (3×20 ml) and dried with magnesium sulfate. Filtration and concentration gave a light yellow oil which was purified by chromatography (ethyl acetate) yielding 162 mg (51%) of 2-{[4-(1,3-dioxo-1,3-dihydroisoindol-2-yl)benzyl]methoxyphosphinoyl methyl}-4-methylpentanoic acid benzyl ester as a yellow solid.

1. customwere refluxed for 1 hour
2. customThe cooled reaction mixture
3. concentrationwas concentrated
4. dissolutionthe residue dissolved in ethyl acetate (100 ml)
5. washThis solution was washed with saturated sodium bicarbonate solution (3×20 ml)
6. dry with materialdried with magnesium sulfate
7. filtrationFiltration and concentration
8. customgave a light yellow oil which
9. customwas purified by chromatography (ethyl acetate)