反应详情

20 g (0.08 mol) of 2,6-dimethyl-N-methoxyacetyl-N-acetonylaniline, 7.5 g (0.09 mol) of O-methyl-hydroxylamine hydrochloride and 9.1 g (0.09 mol) of triethylamine in 100 ml of ethanol were heated under reflux for 5 hours. After distilling off the solvent in vacuo, the residue was partitioned between water/methylene chloride. The organic phase was separated off, dried over sodium sulphate and concentrated. After adding petroleum ether, the residue crystallized. 21 g (94% of theory) of 2,6-dimethyl-N-(2-methoxyimino-prop-1-yl)-N-methoxyacetylaniline of melting point 56°-57° C. were obtained.

1. temperatureunder reflux for 5 hours
2. distillationAfter distilling off the solvent in vacuo
3. customthe residue was partitioned between water/methylene chloride
4. customThe organic phase was separated off
5. dry with materialdried over sodium sulphate
6. concentrationconcentrated
7. additionAfter adding petroleum ether
8. customthe residue crystallized