反应详情

To a solution of 3-(2-chlorophenyl)propanoic acid (200 mg, 1.08 mmol) in N,N-dimethylformamide (20 ml) was added 1-hydroxybenzotriazole monohydrate (187 mg, 1.22 mmol) and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (318 mg, 1.66 mmol). After stirring at room temperature for 10 min, the mixture was treated with the hydrochloride salt of N-[3-(6-methyl-3-azabicyclo[3.1.0]hex-6-yl)phenyl]methanesulfonamide (Preparation 53, 400 mg, 1.32 mmol) and sodium hydrogen carbonate (200 mg, 2.38 mmol). The reaction mixture was stirred at room temperature for 3 d and then concentrated in vacuo. Water (15 ml) was added and the reaction mixture was extracted with ethyl acetate (2×20 ml). The combined organic extracts were washed with water (10 ml), dried (MgSO4), and concentrated in vacuo to afford 510 mg of a light brown oil. Sonication for 5 min at room temperature in dichloromethane (5 ml) followed by filtration afforded the title compound as an off-white solid (124 mg, 27%).

1. stirringThe reaction mixture was stirred at room temperature for 3 d
2. concentrationconcentrated in vacuo
3. additionWater (15 ml) was added
4. extractionthe reaction mixture was extracted with ethyl acetate (2×20 ml)
5. washThe combined organic extracts were washed with water (10 ml)
6. dry with materialdried (MgSO4)
7. concentrationconcentrated in vacuo