HRID2378516

反应详情

EQUATION

反应方程式

HRID 2378516 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A separable flask having a volume of one liter equipped with a nozzle for introducing hydrogen chloride gas was equipped with a stirring device and charged with 50.0 g (301 mmol) of 4-oxo-2-adamantanol, 13.6 g (450 mmol) of paraformaldehyde, 36.2 g (300 mmol) of magnesium sulfate and 650 ml of dried dichloromethane, and it was cooled to 0° C. on an ice bath and stirred. Hydrogen chloride gas generated by mixing 300.7 g (5 mole) of sodium chloride with 700 ml of conc. sulfuric acid was blown thereinto through the nozzle for one hour. After further stirring for 3 hours, magnesium sulfate was filtered, and then the solution was analyzed by gas chromatography to confirm that 4-oxo-2-adamantanol was completely converted and that the intended product was obtained at a selectivity of 93.2%. Hydrogen chloride and dichloromethane were removed, and then refining was carried out by distillation to isolate 55.0 g (256 mmol, yield 85.2%, GC purity 98.8%) of the intended product.

WORKUP

后处理

  1. customA separable flask having
  2. customa volume of one liter equipped with a nozzle
  3. customwas equipped with a stirring device
  4. stirringAfter further stirring for 3 hours
  5. filtrationmagnesium sulfate was filtered
  6. customwas obtained at a selectivity of 93.2%
  7. customHydrogen chloride and dichloromethane were removed
  8. distillationrefining was carried out by distillation
  9. customto isolate 55.0 g (256 mmol, yield 85.2%, GC purity 98.8%) of the intended product