反应详情

To a mixture of 0.8813 g (3.1 mmole) of 4-amino-3-methoxy-benzoic acid benzotriazol-1-yl ester and 8 mL of dry tetrahydrofuran at 0 degrees was added 0.6995 g (3.1 mmole) of 1-methanesulfonyl-piperidin-4-ylamine followed by 0.7842 g (7.75 mmole) of triethylamine. The cooling bath was removed and the mixture stirred at room temperature for 90 hours. Volatiles were removed under reduced pressure and the residue taken up in ethyl acetate, and the organic layer washed twice with 50 mL of 0.5 M sodium carbonate, 50 mL water, and then 50 mL brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure to give 1.0056 g 4-amino-N-(1-ethyl-piperidin-4-yl)-3-methoxy-benzamide.

1. customThe cooling bath was removed
2. customVolatiles were removed under reduced pressure
3. washthe organic layer washed twice with 50 mL of 0.5 M sodium carbonate, 50 mL water
4. dry with material50 mL brine, dried over anhydrous sodium sulfate
5. concentrationconcentrated under reduced pressure