反应详情

A solution of compound 4 (223 mg, 1.0 mmol) in dimethylformamide (2.5 mL) under argon at room temperature was treated with 3,3-dimethylbutyl amine (111 mg, 1.1 mmol), ethyl-3-(3-dimethylamino)-propylcarbodiimide hydrochloride (327 mg, 1.1 mmol) and hydroxybenzotriazole monohydrate (148 mg, 1.1 mmol) and stirred overnight. The reaction mixture was diluted with ethyl acetate and washed with 10% citric acid, water, dilute sodium bicarbonate, water and brine, dried (anhydrous mnagnesium sulfate) and concentrated to give an oil. Flash chromatography on silica gel and elution with ethyl acetate/hexanes (1:4) gave an oil (274 mg) that slowly solidified, mp 75-76.5° C. Analysis calculated for C18H30N2O2: C, 70.55; N, 9.87; N, 9.14. Found: C, 70.46; H, 10.06; N, 9.02.

1. washwashed with 10% citric acid, water, dilute sodium bicarbonate, water and brine
2. dry with materialdried (anhydrous mnagnesium sulfate)
3. concentrationconcentrated
4. customto give an oil
5. washFlash chromatography on silica gel and elution with ethyl acetate/hexanes (1:4)