反应详情

温度

60 °C

The product from step (b) (2.79 g) in dry THF (80 ml) was treated with triphenylphosphine (3.47 g) and water (12 ml) and the mixture heated at 60° C. for 2 h. The reaction mixture was cooled, poured into water, and extracted with ethyl acetate which was washed with water and dried (MgSO4). The solvent was evaporated and the residue purified by chromatography (silica, ethyl acetate and then 10% 7M ammonia in methanol/dichloromethane as eluent) to give an oil. This was dissolved in ethanol (10 ml), treated with fumaric acid (70.3 mg) and heated until a clear solution was obtained. The mixture was evaporated and the residue triturated with ether to give after filtration and drying in vacuo the final compound (222 mg).

1. temperatureThe reaction mixture was cooled
2. extractionextracted with ethyl acetate which
3. washwas washed with water
4. dry with materialdried (MgSO4)
5. customThe solvent was evaporated
6. customthe residue purified by chromatography (silica, ethyl acetate
7. custom10% 7M ammonia in methanol/dichloromethane as eluent) to give an oil
8. temperatureheated until a clear solution
9. customwas obtained
10. customThe mixture was evaporated
11. customthe residue triturated with ether
12. customto give
13. filtrationafter filtration
14. dry with materialdrying in vacuo the final compound (222 mg)