反应详情

温度

10 °C

N-Benzyloxycarbonyl-L-valine (2.02 g, 8.0 mmol), 4-dimethylaminopyridine (100 mg, 0.8 mmol), and), and dicyclohexylcarbodiimide (2.04 g, 9.9 mmol, is 20 mL CH2Cl2) were added to 2-methyl-1,2-propanediol (12.2 mmol) in 30 mL dry CH2Cl2, with cooling in an ice bath. DMF (5 mL) was added. After stirring for 5 h at 10° C., the reaction mixture was filtered, concentrated, and then redissolved in ethyl acetate. The organic solution was washed with saturated NaCl, dried over anhydrous Na2SO4, and concentrated. Flash column chromatography (silica, 2/1 petroleum ether-ethyl acetate) gave 2.3 g of the title compound.

1. temperaturewith cooling in an ice bath
2. filtrationthe reaction mixture was filtered
3. concentrationconcentrated
4. dissolutionredissolved in ethyl acetate
5. washThe organic solution was washed with saturated NaCl
6. dry with materialdried over anhydrous Na2SO4
7. concentrationconcentrated