反应详情

Into a round-bottom flask of the volume of 100 ml are transferred 50 ml dioxane and the solvent is cooled to 5° C. Subsequently 8.1 g (0.18 mole) dimethylamine is absorbed in the solvent at the temperature of 5-10° C. in 20 minutes. To the solution of dimethylamine, 10.2 g (0.1 mole) of [1,4]-dioxane-2-one are added at the same temperature in 5 minutes and the reaction mixture is stirred at room temperature for 2 hours. After the reaction period, the solvent is evaporated in vacuo at the temperature of 50° C. in one hour. Thus 14.1 g (95.9%) of the title product are obtained, which has the purity of 98% as determined by gas chromatography. Optionally the product can be purified by distilling in vacuo (boiling temperature 130-135° C./13 Pa). The raw product is directly suitable for the preparation of 2-chloroethoxy-acetic acid-N,N-dimethyl-amide.

1. customInto a round-bottom flask of the volume of 100 ml are transferred
2. customAfter the reaction period
3. customthe solvent is evaporated in vacuo at the temperature of 50° C. in one hour