反应详情

A mixture of Compound 3 (18.1g, 100 mmol) and hydroxylamine hydrochloride (7.0 g, 101 mmol) in 100 mL of anhydrous methanol was refluxed under nitrogen for 2 hours. The reaction mixture was cooled, concentrated and partitioned between water and dichloromethane. The dichloromethane layer was dried with anhydrous sodium sulfate, filtered and concentrated to yield compound 4 as a dark yellow-orange oil (14.1 g, 93.3 mmol, 93%). GC/MS, m/z=151 at tR=8.30 min (100%). LC/MS, [M+H]=152.

1. temperaturewas refluxed under nitrogen for 2 hours
2. temperatureThe reaction mixture was cooled
3. concentrationconcentrated
4. custompartitioned between water and dichloromethane
5. dry with materialThe dichloromethane layer was dried with anhydrous sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated