反应详情

A suspension of Example 58B (1 g, 4.08 mmol) and chloroformamidine hydrochloride (1.17 g, 10.2 mmol) in diglyme (40 mL) was heated to 130° C. for 15 hours. The mixture was cooled to room temperature, diluted with water, and extracted twice with ethyl acetate. The combined extracts were washed with brine, dried (MgSO4), filtered, and concentrated. The residue was further concentrated under a stream of nitrogen, and purified by silica gel chromatography with 5 to 7% methanol/dichloromethane to provide 0.26 g of the desired product. MS (ESI(+)) m/e 288 (M+H)+.

1. extractionextracted twice with ethyl acetate
2. washThe combined extracts were washed with brine
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated
6. concentrationThe residue was further concentrated under a stream of nitrogen
7. custompurified by silica gel chromatography with 5 to 7% methanol/dichloromethane