反应详情

温度

65 °C

(3R)-6-Carboxy-5-oxo-1-thia-4-azacyclotridecane-3-carboxylic acid (1.71 g, 5.64 mmol) is dissolved in pyridine (20 ml) and piperidine (0.096 g, 1.13 mmol) is added followed by paraformaldehyde (0.25 g, 8.46 mmol). The mixture is heated to 65° C. and stirred for 2 hours. The mixture is cooled to room temperature, poured into 6N hydrochloric acid (100 ml) and extracted with ethyl acetate (2×100 ml). The combined extracts are washed with brine (1×100 ml), dried (MgSO4) and solvent is evaporated to give (3R)-6-methylidene-5-oxo-1-thia-4-azacyclotridecane-3-carboxylic acid, m.p. 184°-186° C.

1. temperatureThe mixture is cooled to room temperature
2. extractionextracted with ethyl acetate (2×100 ml)
3. washThe combined extracts are washed with brine (1×100 ml)
4. dry with materialdried (MgSO4) and solvent
5. customis evaporated