反应详情

2-{[1-(tert-butoxycarbonyl)piperidin-4-yl]amino}-6-chlorobenzoic acid Sodium triacetoxyborohydride (3.09 g, 14.6 mmol) was added to a solution of 2-amino-6-chlorobenzoic acid (1.00 g, 5.83 mmol) and N-(t-butoxycarbonyl)-4-piperidone (2.32 g, 11.7 mmol) in dichloroethane (20 mL) at room temperature. After 5 h, the reaction was quenched with saturated aqueous ammonium chloride. This mixture was separated and extracted with ethyl acetate (3×). After drying over sodium sulfate, the solution was filtered and evaporated to give the crude product. This was purified by chromatorgraphy (silica gel, 0 to 15% methanol in methylene chloride gradient elution), which gave the title compound contaminated with some ketone starting material (3.60 g). MS 335.1 (M+1).

1. customthe reaction was quenched with saturated aqueous ammonium chloride
2. customThis mixture was separated
3. extractionextracted with ethyl acetate (3×)
4. dry with materialAfter drying over sodium sulfate
5. filtrationthe solution was filtered
6. customevaporated
7. customto give the crude product
8. customThis was purified by chromatorgraphy (silica gel, 0 to 15% methanol in methylene chloride gradient elution), which