反应详情

9.25 g (40 mmoles) of N-mesyl-O-(p-methoxybenzyl)hydroxylamine prepared as described in Reference Example 5 was added to sodium methoxide (prepared from 150 ml of absolute methanol and 1.2 g of sodium metal), and 6 g of benzyl chloride was then added to the mixture. The resulting mixture was heated under refluxing for 3 hours. The solvent was distilled off, and 150 ml of ethyl acetate and 50 ml of water were added to the residue. The organic layer was separated, dried over anhydrous sodium sulfate and concentrated to obtain 8.4 g (65.6% yield) of N-benzyl-N-mesyl-O-(p-methoxybenzyl)hydroxylamine having a melting point of 85°-87° C.

1. additionwas then added to the mixture
2. temperatureThe resulting mixture was heated
3. temperatureunder refluxing for 3 hours
4. distillationThe solvent was distilled off
5. addition150 ml of ethyl acetate and 50 ml of water were added to the residue
6. customThe organic layer was separated
7. dry with materialdried over anhydrous sodium sulfate
8. concentrationconcentrated