反应详情

Propene was passed for 30 minutes at room temperature into a solution of 15.0 g (52 mmol) of methyl 2-chloro-3-hydroxyiminomethyl-4-methylsulfonylbenzoate and 200 ml of dichloromethane. After 1.6 g of sodium acetate had been added, 42.8 ml of sodium hypochlorite solution were added dropwise at room temperature while simultaneously passing in propene. Propene was subsequently passed in for a further 15 minutes at room temperature. After the mixture had been refluxed for 3 hours, it was stirred for 12 hours at room temperature, propene was again passed in for 5 hours under reflux, and the mixture was stirred for a further 12 hours at room temperature. After the phases had been separated, the organic phase was washed with water, dried and concentrated. This gave 15.5 g (89% of theory) of methyl 2-chloro-(5-methyl-4,5-dihydroisoxazol-3-yl)-4-methylsulfonylbenzoate.

1. customwas subsequently passed in for a further 15 minutes at room temperature
2. temperatureAfter the mixture had been refluxed for 3 hours
3. customwas again passed in for 5 hours
4. temperatureunder reflux
5. stirringthe mixture was stirred for a further 12 hours at room temperature
6. customAfter the phases had been separated
7. washthe organic phase was washed with water
8. customdried
9. concentrationconcentrated