反应详情

To a suspension of (S)-2-nitro-6-(piperidin-3-ylmethoxy)benzonitrile hydrochloride (Example 1d, 9.8 g, 32.92 mmol) in CH2Cl2 (550 mL) and DMF (50 mL) was added triethylamine (9.2 mL, 65.84 mmol). After being stirred at room temperature for 5 min., a solution of butyric acid (3.33 mL, 36.21 mmol), EDCI (6.94 g, 36.21 mmol) and HOBt (4.89 g, 36.21 mmol) in DCM (50 mL) was added, and the reaction mixture was then stirred at room temperature overnight. The resulting mixture was diluted with CH2Cl2, washed with 0.5 N HCl, water, NaHCO3 and brine, dried over MgSO4, filtered and evaporated to give the crude product as a light brown gel, used as this in the next step. MS 332 (MH+).

1. stirringthe reaction mixture was then stirred at room temperature overnight
2. washwashed with 0.5 N HCl, water, NaHCO3 and brine
3. dry with materialdried over MgSO4
4. filtrationfiltered
5. customevaporated