反应详情

To a suspension of L-proline benzyl ester hydrochloride (3.37 g) in dichloromethane (60 ml) were added N-methylmorpholine (1.54 ml), N-(t-butoxycarbonyl)-L-proline (3.00 g), HOBt (2.08 g) and water-soluble carbodiimide hydrochloride (2.95 g) in order, followed by stirring for 1 hour. After stirring at room temperature for 17 hours, the reaction mixture was poured into ethyl acetate, washed with 1N hydrochloric acid, a saturated aqueous solution of sodium bicarbonate and saturated brine in order, dried over anhydrous magnesium sulfate, and concentrated. The residue was purified by silica gel column chromatography (eluate; hexane-ethyl acetate) to give 5.00 g of the title compound.

1. stirringAfter stirring at room temperature for 17 hours
2. washwashed with 1N hydrochloric acid
3. dry with materiala saturated aqueous solution of sodium bicarbonate and saturated brine in order, dried over anhydrous magnesium sulfate
4. concentrationconcentrated
5. customThe residue was purified by silica gel column chromatography (eluate; hexane-ethyl acetate)