HRID1706870
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of 1.48 g of the 2-chloromethyl-5-methyl-4-isoxazolin-3-one thus obtained in 30 ml of acetone were added 2.52 g of crystalline potassium O,O-di-n-propyl dithiophosphate, and the resulting mixture was then stirred for 1 hour at ambient temperature. The acetone was then evaporated off and the residue was purified by column chromatography through silica gel eluted with a 20:1 by volume mixture of benzene and acetone. There were obtained 2.39 g (73.5% of theory) of O,O-di-n-propyl S-(5-methyl-3-oxo-4-isoxazolin-2-ylmethyl) phosphorodithioate, in the form of a pale yellow oil, n20D =1.5314.
WORKUP
后处理
- customThe acetone was then evaporated off
- customthe residue was purified by column chromatography through silica gel
- washeluted with a 20:1 by volume mixture of benzene and acetone