【摘要】 为解决因采用高温反应所引起的9,10-二氢-9-氧杂-10磷杂菲-10氧化物(DOPO),产品质量问题,首先采用在170～180℃下、8h反应的一步法合成中间产物6-氯-6氢-二苯并[c,e][1,2]-氧杂膦(CDOP),以简化反应过程,并减少副反应的发生,然后在过量水存在的条件下充分进行水解反应,并采用有机溶剂对水解产物进行提纯,以避免使用高真空;最后在116～125℃的低温进行的脱水反应,以防止产物发生分解,从而得到高纯度、高收率的产品DOPO。更多还原

【Abstract】 During synthesize of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, one-step method was chosen to prepare 6-chloro-6H-dibenzo[c,e][1,2] oxaphosphinine (CDOP) at 170～180 ℃ in 8 hours, which reduce the time of reaction and simplify the process of reaction; Then CDOP was hydrolyzed rapidly in excessive water. and the intermediate product was purified by extracted with organic solvent to avoid using the high vacuum. In the last step, DOPO with high yield and purity was made through dehydration in 116～125 ℃.更多还原