HRID1578925

反应详情

EQUATION

反应方程式

HRID 1578925 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

With stirring and reflux cooling, 183 g (1 mole) of adipic acid chloride were added to a solution, kept at 120°C., of 168.6 g (1.1 moles) of cyclooctylisocyanate and 162 ml (2 moles) of pyridine in 500 ml of xylene. After 3 hours' reaction time, cooling was effected, followed by filtering off from the separated pyridine hydrochloride. The filtrate was first freed from solvent under reduced pressure and, finally, was distilled in a high vacuum. 158.2 g (60% of the theory) of 3-cyclooctyl-2,3,4,5,6,7-hexahydrocyclopenta[e]-1,3-oxazine-2,4-dione of the boiling point 172°-174°C/0.3 mm Hg were obtained when solidified to give a colorless crystal mass of the melting point 48°-51°C.

WORKUP

后处理

  1. temperaturereflux
  2. temperaturecooling
  3. customAfter 3 hours' reaction time
  4. temperaturecooling
  5. filtrationby filtering off from the separated pyridine hydrochloride
  6. distillationfinally, was distilled in a high vacuum