3,3'-二(N-羟基偕胺肟基)二呋咱基醚合成及歧化反应

以3-氰基-4-硝基呋咱为原料,经分子间醚化、加成、重氮化、双肟化得到3,3'-二(N-羟基偕胺肟基)二呋咱基醚(DOFOF),总收率达51.0%,用IR、1H NM R、13C NM R、元素分析等进行了结构表征。初步优化了双肟化工艺,确定了最佳反应条件:反应温度20℃,n(DCFOF)n(NH2O H·HC l)n(KO H)=144。发现了DO FO F在碱性条件下易发生歧化反应,分离鉴定了歧化产物3,3'-二偕胺肟基二呋咱基醚,并从理论上提出了可能的歧化反应机理。

TCC&TCS对废水处理中生物相的急性毒性试验

研究了TCC(3,4,4′-Trichlorocarbanilde)、TCS(2,2,4′-Trichloro-2′-hydroxydiphenyl)对废水生物处理中的原生动物的急性毒性作用。结果表明:TCC对原生动物的48h半数致死浓度LC_(50)为25000μg/L,TCS48hLC_(50)为23000μg/L,TCC＆ TCS浓度与原生动物的半数致死时间LT_(50)呈明显的负相关;TCC ＆ TCS对原生动物的最大无作用浓度分别为15mg/L和11mg/L,这提示污染源排放的废水到达曝气池时TCC ＆ TCS的含量应低于15mg/L和11mg/L。

Preparation and Purification of Halogenated Hydroxydiphenyl Ethers

As a good antimicrobial active ingredient, 2,4,4′ trichloro 2′ hydroxydiphenyl ether has been already commercially available since 1970s. For this paper halogenated hydroxydiphenyl ethers were prepared and purified, and their analytical conditions by HPLC were studied. Further purification of 2,4,4′ trichloro 2′ hydroxydiphenyl ether was also studied. The adsorption ability of different decolourants, e.g. alumina and bentonite, for each component in crude product of 2,4,4′ trichloro 2′ hydroxydiphenyl ether was varied. 2,4,4′ trichloro 2′ hydroxydiphenyl ether might be adsorbed by active carbon. The colored impurities might be adsorbed by alumina. The colorless impurities might be adsorbed by bentonite.

Crystal Structure of Bis(3-hydroxy-2-pyridyl)disulfide

C_(10)H_8N_2O_2S_2, Mr=252. 32,monoclinic,P2_(1/c),a=7.165(5).b=7.659(3),c=19.543(8)A,β=96. 76(5)°,V=1065.0(9) A,Z=4,D_c=1. 57 g/cm￣3.The structure was solved by direct methods and refined to final R(R_w)=0.051(0.057) for 1446 observed reflections with I≥3σ(Ⅰ).The sulfur-sulfur bond length is found to be 2. 019(2) A with a dihedral angle CSSC of 93.29°.