反应详情

A solution of compound Compound 2 (5.0 g, 20.2 mmol) from step (b) of Example 1 dissolved in chloroform (30 ml) was added drop wise to a solution of dihexylamine (4.5 g, 24.2 mmol) in chloroform (20 ml). The combined mixture was stirred at room temperature for 2 hours. The reaction mixture was then washed with water (2×, 50 ml) and brine (1×, 50 ml). The organic layer was then dried with sodium sulfate and evaporated. The residue thus obtained was suspended in ca. 5 ml hot ethyl acetate and this solution was then slowly added to 40 ml hexane. The white solid that precipitated was filtered and the filtrate evaporated to dryness to provide 7.76 g (97%) of Compound 20 as a syrupy liquid, Rf=0.43 (30% ethyl acetate in hexane). The structure of this compound 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 then dried with sodium sulfate
3. customevaporated
4. customThe residue thus obtained
5. customThe white solid that precipitated
6. filtrationwas filtered
7. customthe filtrate evaporated to dryness