反应详情

A solution of Compound 2 (2.5 g, 10 mmol) in chloroform (15 ml) was added drop wise to a solution of piperidine (1.7 g, 20.0 mmol) in chloroform (10 ml). The combined mixture was stirred at room temperature for 1 hour. The reaction mixture was then washed with water (2×, 50 ml) and brine (1×, 50 ml). The organic layer was dried with sodium sulfate and evaporated. The sticky white solid thus obtained was dissolved in ca. 5 ml of hot ethyl acetate and this solution was then slowly added to 40 ml hexane. The white solid that precipitated was collected, washed with hexane and dried to yield 2.2 g (74%) of Compound 3, Rf=0.28 (30% ethyl acetate in hexane). The structure of Compound 3 is given below:

1. washThe reaction mixture was then washed with water (2×, 50 ml) and brine (1×, 50 ml)
2. dry with materialThe organic layer was dried with sodium sulfate
3. customevaporated
4. customThe sticky white solid thus obtained
5. customThe white solid that precipitated
6. customwas collected
7. washwashed with hexane
8. customdried