HRID1578925
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturereflux
- temperaturecooling
- customAfter 3 hours' reaction time
- temperaturecooling
- filtrationby filtering off from the separated pyridine hydrochloride
- distillationfinally, was distilled in a high vacuum