摘要
通过 4 氯 5 环戊氧基 2 氟异氰酸苯酯与 2 羟基 3 甲基 3 丁烯腈发生加成环化反应制得除草剂 3 (4 氯 5 环戊氧基 2 氟苯基 ) 4 亚胺基 5 异丙叉基恶唑烷 2 酮。反应分两阶段进行 ,首先在冰水浴中向 2 羟基 3 甲基 3 丁烯腈中滴加 4 氯 5 环戊氧基 2 氟异氰酸苯酯甲苯溶液 ,然后升至室温反应 4h。优化的反应条件为 :三乙胺作催化剂 ,n(4 氯 5 环戊氧基 2 氟异氰酸苯酯 )∶n(2 羟基 3 甲基 3 丁烯腈 ) =1 0∶1 2 ,加料方式为滴加 4 氯 5 环戊氧基 2 氟异氰酸苯酯甲苯溶液 ,第二阶段反应在室温下进行。反应条件优化以后 ,产品收率可由 39%提高到 5 6 %。产品结构用CIMS、1HNMR进行了确定。分离了其中一个副产物 ,并对其结构进行了鉴定。
Herbicide 3 (4 chloro 5 cyclopentyloxy 2 fluorophenyl) 4 imine 5 isopropylideneoxazolidine 2 one(Ⅰ) is obtained through the addition cyclization of 4 chloro 5 cyclopentyloxy 2 fluorophenylisocyanate(Ⅱ) and 2 hydroxy 3 methyl 3 butenenitrile(Ⅲ).The reaction is carried out in two steps.At first,under the cooling of ice water mixture,the toluene solution containing Ⅱ is dropped into Ⅲ.Then the temperature is raised to room temperature and the reaction proceeds for 4 h.Triethylamine is used as catalyst.Molar ratio of Ⅱ to Ⅲ is 1 0∶1 2.Under the above optimized conditions,yield of the product(Ⅰ) can be raised from 39% to 56%.Structure of the product is confirmed by CIMS and 1 HNMR .A side-reaction product is separated,and its structure is identified. Key words:3 (4 chloro 5 cyclopentyloxy 2 fluorophenyl) 4 imine 5 isopropylideneo xazolidine 2 one;addition cyclization;herbicide?00085, China E mail: yuanbl@hotmail.com;2. Institute of Water Technologies, Shenzhen Water Supply (group) Co., LTD., Shenzhen 518031, China)Abstract:This paper studied the efficiency of algae removal by ferrate from two kinds of raw water which were collected from Donghu and Tiegang reservoir respectively. The experimental results showed that the removal efficiency of algae reached about 95% only through PAC coagulation when the raw water was extracted from Donghu reservoir in which most of algae was Chlorella. But dealing with Tiegang raw water in which the majority of algae were Oscillatoria, terrate was used as pre oxidant coupling with PAC coagulation not only using PAC to flocculate and the efficiency of algae removal could be up to 97 85%. However this treatment method using ferrate as pre oxidant overmatched the traditional method prechlorination for algae removal.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2001年第2期121-123,共3页
Fine Chemicals
