反应详情

The impure 1,1-dichloro-7-oxaspiro[3.5]nonan-2-one from Step B was stirred with zinc (150 mg; 2.30 mmol) and 5 mL of acetic acid/water (1:1) for 4 hours. The mixture was stored at −20° C. for 1 day, diluted with ether (20 mL) and filtered through a pad of Celite®. The solution was neutralized with aqueous sodium bicarbonate solution and extracted into ether (5×20 mL). The combined ether extracts were dried (sodium sulfate), filtered and concentrated under reduced pressure. The material was purified by chromatography on silica gel, eluting with 1:1 ethyl acetate/hexane to give the product as a colorless oil (61 mg).

1. filtrationfiltered through a pad of Celite®
2. extractionextracted into ether (5×20 mL)
3. dry with materialThe combined ether extracts were dried (sodium sulfate)
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customThe material was purified by chromatography on silica gel
7. washeluting with 1:1 ethyl acetate/hexane