反应详情

The compound (281 mg) obtained in Example 84-5 was dissolved in dichloromethane (6.0 ml) and added with diisopropylethylamine (310 μl) at room temperature under a nitrogen atmosphere. The solution was added with tritylchloride (310 mg) under ice-cooling and the whole was stirred at room temperature for 4 hours. After completion of the reaction, methanol was added thereto. The solvent was distilled off under reduced pressure and the residue was diluted with chloroform and added with water. The aqueous layer was subjected to extraction with chloroform. The combined organic layer was washed with a saturated saline solution and dried with anhydrous sodium sulfate. After filtration, the solution was concentrated and evaporated to dryness under reduced pressure and the residue was purified through silica gel column chromatography (chloroform/methanol), thereby obtaining the subject compound (217 mg) as a yellow oily substance.

1. temperaturecooling
2. additionwas added
3. distillationThe solvent was distilled off under reduced pressure
4. additionthe residue was diluted with chloroform
5. additionadded with water
6. extractionThe aqueous layer was subjected to extraction with chloroform
7. washThe combined organic layer was washed with a saturated saline solution
8. dry with materialdried with anhydrous sodium sulfate
9. filtrationAfter filtration
10. concentrationthe solution was concentrated
11. customevaporated to dryness under reduced pressure
12. customthe residue was purified through silica gel column chromatography (chloroform/methanol)