反应详情

To a solution of (R)—N-sec-butyl-3-(piperazin-1-ylmethyl)benzamide (5.08 mmol, 1.4 g), 4-amino-3-fluorobenzoic acid (5.08 mmol, 0.789 g) and triethylamine (15.25 mmol, 2.126 mL, 1.543 g) in dichloromethane (80 mL) was added 1-propanephosphonic acid cyclic anhydride (7.63 mmol, 2.270 mL, 2.426 g, 50% solution in ethyl acetate). The reaction mixture was stirred for 1 hour then was diluted with ethyl acetate and potassium carbonate (aqueous). The organic layer was separated, dried (magnesium sulfate) and concentrated under reduced pressure. Chromatography on silica (eluting with ethyl acetate to ethyl acetate/methanol (5%)) gave the intermediate (R)-3-((4-(4-amino-3-fluorobenzoyl)piperazin-1-yl)methyl)-N-sec-butylbenzamide (1.2 g).

1. customThe organic layer was separated
2. dry with materialdried (magnesium sulfate)
3. concentrationconcentrated under reduced pressure