反应详情

To the solution obtained in step (b) above was added dropwise the isoxazolinone solution obtained in step (a) above, with stirring, over a period of 5 minutes at ambient temperature. The mixture was then stirred for a further 30 minutes, also at ambient temperature. After distilling off the solvent, 100 ml of benzene and 25 ml of water were added to the residue and the benzene phase was washed, in turn, with 25 ml of a 5% w/w aqueous sodium bicarbonate solution and twice with 100 ml of a saturated aqueous sodium chloride solution. The benzene solution was then dried over anhydrous sodium sulphate and the solvent was distilled off. The residue was then purified as described in step (b) of Example 3, affording 28.5 g (85.8% of theory) of O,O-diethyl S-(4-chloro-5-methyl-3-oxo-4-isoxazolin-2-ylmethyl) phosphorodithioate, in the form of a yellow oil, n20D =1.5457.

1. stirringThe mixture was then stirred for a further 30 minutes, also at ambient temperature
2. distillationAfter distilling off the solvent, 100 ml of benzene and 25 ml of water
3. additionwere added to the residue
4. washthe benzene phase was washed, in turn, with 25 ml of a 5% w/w aqueous sodium bicarbonate solution and twice with 100 ml of a saturated aqueous sodium chloride solution
5. dry with materialThe benzene solution was then dried over anhydrous sodium sulphate
6. distillationthe solvent was distilled off
7. customThe residue was then purified