反应详情

50ELH4 (0.11 g, 0.49 mmol, 1.0 eq.) was transferred to a 4 ml vial and dissolved in dichloromethane. 63ELH19 (0.089 mg, 1.0 eq.) was added and the vial was sealed and the reaction shaken for 20 h. The product was extracted in distilled water (made basic with potassium carbonate, pH 10) and dichloromethane. Dried with sodium sulfate and concentrated. Purified by HPLC. The extraction, drying and concentration was repeated and the product dissolved in dichloromethane (1 ml) and HCl (1 eq., 2 M in ether) is added. This mixture was added drop-wise to an excess of heptane whereupon the salt precipitated. Yield 31.1 mg (16%), UV/MS: 94/100 (M+ 385), tr (A, MS) 2.573.

1. customthe vial was sealed
2. extractionThe product was extracted in distilled water (made basic with potassium carbonate, pH 10)
3. dry with materialDried with sodium sulfate
4. concentrationconcentrated
5. customPurified by HPLC
6. extractionThe extraction
7. customdrying
8. concentrationconcentration
9. dissolutionthe product dissolved in dichloromethane (1 ml)
10. customprecipitated