反应详情

温度

0 °C

Add the product from step 2 (0.35 g, 1.28 mmol) in methylene chloride (20 mL) to a mixture of triethyl amine (0.605 mL, 4.34 mmol) and hexahydro-2H-1,4-diazepine (also known as homopiperazine) (0.326 g, 3.25 mmol) in methylene chloride (7 mL) cooled to 0° C. over 5 min. Stir the reaction mixture for 15 min at 0° C. Add aqueous HCl (25 mL, 1N) to the reaction mixture. Filter the solid and recrystallize from absolute ethanol to give the title compound (0.33 g, 69%) as light yellow needles. Rf=0.54 (5% MeOH in methylene chloride (v/v), 0.2% ammonium hydroxide buffer).

1. filtrationFilter the solid
2. customrecrystallize from absolute ethanol