反应详情

A solution of the diethyl ester product from part (b) (4.0 g., 10.9 mmole) in dry dichloromethane (8.0 ml.) is treated with trimethylsilylbromide (3.6 ml., 27.3 mmole) and stirred at room temperature under argon for 22 hours. The mixture is evaporated to dryness (0.5 mm. of Hg) and the residue taken up in dichloromethane (30 ml.)-water (5 ml.) and stirred vigorously for 15 minutes. The organic phase is separated, dried (Na2SO4), and evaporated. The crystalline residue is triturated with ethyl ether to give 3.20 g. of (6-phthalimidohexyl)phosphinic acid as a white solid; m.p., 159°-160°. Tlc (isopropanol-conc. NH4OH-water; 7:2:1) shows a single spot at Rf =0.20.

1. customThe mixture is evaporated to dryness (0.5 mm. of Hg)
2. stirringstirred vigorously for 15 minutes
3. customThe organic phase is separated
4. dry with materialdried (Na2SO4)
5. customevaporated
6. customThe crystalline residue is triturated with ethyl ether
7. customto give 3.20 g
8. customm.p., 159°-160°