反应详情

温度

25 °C

434.1 g (4.0 mol) of methyl chloroacetate are initially introduced and stirred at 25° C. 756.3 g (4.2 mol) of 30% strength sodium methoxide solution are added dropwise in the course of 2.5 h such that a reaction temperature of 65° C. is not exceeded. After the addition, stirring is continued at reflux temperature for a further 3 h. 407.5 g of methanol are then separated from the reaction mixture by distillation. 480.8 g (8 mol) of isopropanol are added to the residue and the mixture is heated under reflux. In the course of this, methanol is removed through a 0.5 m long Multifil column at a reflux ratio of approximately 1:1 (291.9 g of distillate). After 6.5 h, the conversion of the methyl methoxyacetate to the isopropyl methoxyacetate is >98%. After cooling, the reaction mixture is filtered off with suction and the residue is washed with 450 g of isopropanol. A residue of 412.1 g and a liquid phase (filtrate and wash liquid) of 969.9 g are obtained. The liquid phase is fractionated through a 0.5 m long Multifil column. Isopropyl methoxyacetate (405.0 g, yield 77%) with an organic purity of >99%, a chlorine content of 10 ppm and a water content of <0.05% is obtained as the main fraction.

1. additionAfter the addition
2. stirringstirring
3. temperatureat reflux temperature for a further 3 h
4. custom407.5 g of methanol are then separated from the reaction mixture by distillation
5. temperaturethe mixture is heated
6. temperatureunder reflux
7. customIn the course of this, methanol is removed through a 0.5 m long Multifil column at a reflux ratio of approximately 1:1 (291.9 g of distillate)
8. temperatureAfter cooling
9. filtrationthe reaction mixture is filtered off with suction
10. washthe residue is washed with 450 g of isopropanol
11. washA residue of 412.1 g and a liquid phase (filtrate and wash liquid) of 969.9 g
12. customare obtained