反应详情

To a solution of 1-methoxy-piperidin-4-one [prepared according to Journal of Organic Chemistry (1961), 26, 1867-74] (258 g, 2.0 mol) and triethylamine (305.2 ml, 221.9 g, 4.4 mol) in methanol (3000 ml) was added hydroxylamine hydrochloride (277.6 g, 4.0 mol), and the reaction mixture heated at reflux for 1.5 hours. The solvent was evaporated, the residue diluted with diethyl ether and the suspension filtered. The filtrate was washed with water and brine, dried over sodium sulfate and concentrated. Yield: 286.25 g of 1-methoxy-piperidin-4-one oxime as a colorless, viscous oil. This material was used without further purification in the next step.

1. temperaturethe reaction mixture heated
2. temperatureat reflux for 1.5 hours
3. customThe solvent was evaporated
4. additionthe residue diluted with diethyl ether
5. filtrationthe suspension filtered
6. washThe filtrate was washed with water and brine
7. dry with materialdried over sodium sulfate
8. concentrationconcentrated
9. customThis material was used without further purification in the next step