反应详情

A solution of (8-nitromethyl-1,4-dioxa-spiro[4.5]dec-8-yl)-acetic acid methyl ester (5.34 g, 19.5 mmol) in 35 mL of methanol was purged with nitrogen. A portion of about 430 mg of Raney 2800 nickel was added. The reaction mixture was purged with hydrogen and a positive pressure of hydrogen was maintained overnight using a balloon. Then, the final mixture was purged with nitrogen and filtered through a pad of celite washing with methanol. The filtrate was concentrated to afford 1,4-dioxa-10-aza-dispiro[4.2.4.2]tetradecan-11-one (3.95 g, 96%) as a white solid.

1. customThe reaction mixture was purged with hydrogen
2. temperaturea positive pressure of hydrogen was maintained overnight
3. customThen, the final mixture was purged with nitrogen
4. filtrationfiltered through a pad of celite
5. washwashing with methanol
6. concentrationThe filtrate was concentrated