反应详情

温度

60 °C

The resulting oil from Step 2 was dissolved in wet tetrahydrofuran (225 ml) and was treated with triphenylphosphine (53.3 g, 203 mmol). The reaction was heated at 60° C. and stirred for 4 h. The solvent was removed under vacuum, the residue re-dissolved into 2N hydrochloric acid (1000 ml) and the aqueous layer was extracted with ethyl acetate (3 times 700 ml). The aqueous phase was basified with a 2N sodium hydroxide solution and extracted with dichloromethane (3 times 1000 ml). The combined organic layers were washed with brine, dried over sodium sulfate, filtered and concentrated under vacuum. The crude material was purified by chromatography (8% 7N ammonia in methanol/DCM) to give the title compound as a yellow oil (17 g).

1. customThe solvent was removed under vacuum
2. dissolutionthe residue re-dissolved into 2N hydrochloric acid (1000 ml)
3. extractionthe aqueous layer was extracted with ethyl acetate (3 times 700 ml)
4. extractionextracted with dichloromethane (3 times 1000 ml)
5. washThe combined organic layers were washed with brine
6. dry with materialdried over sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated under vacuum
9. customThe crude material was purified by chromatography (8% 7N ammonia in methanol/DCM)