HRID1589414

反应详情

EQUATION

反应方程式

HRID 1589414 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

340 g of 2-chloro-2-(2,2-dimethyl-1,3-dioxolan-4-yl)ethanol is dissolved in 1.5 l of absolute ether. At 5° C., a total of 130 g of pulverized potassium hydroxide is added under intensive agitation within 30 minutes, while the temperature is maintained between 5° and 15° C. by cooling. The suspension is then heated at 40° C. for 2 hours under gentle refluxing. After heater and agitator have been turned off, the phases begin to separate. After allowing the mixture to stand overnight, it is vacuum-filtered over kieselguhr. The residue is extracted with ether. The combined ether extracts are concentrated over a 60 cm Vigreux column. The residue (260 g) is distilled under vacuum, during which step 180 g of a colorless liquid passes over; this liquid is fractionated, yielding 2-(2,2-dimethyl-1,3-dioxolan-4-yl)ethylene oxide at 65° C./13 mm.

WORKUP

后处理

  1. temperatureis maintained between 5° and 15° C.
  2. temperatureby cooling
  3. customto separate
  4. filtrationit is vacuum-filtered over kieselguhr
  5. extractionThe residue is extracted with ether
  6. concentrationThe combined ether extracts are concentrated over a 60 cm Vigreux column
  7. distillationThe residue (260 g) is distilled under vacuum, during which step 180 g of a colorless liquid