- Palladium(II) benzisothiazolinate (bit) complexes with amino-, acetylamino-, heterocyclic and phosphine co-ligands. Crystal structure of [Pd(bit)2(κ2-dppe)]·2EtOH
-
Abstract A series of square-planar palladium(II) benzisothiazolinate (bit) of the general type [Pd(bit)2L2] have been prepared and characterized by analytical and spectroscopic methods. Two synthetic routes have been employed, namely reactions of [Pd(bit)2]·H2O with two equivalents of ligands (L = amine, amide, phosphine) or nucleophile displacement of chloride by benzisothiazolinate starting from trans-[PdCl2L2]. Both routes afford the new complexes in good yields as easily isolated, air and moisture stable, colored solids. The precursor, [Pd(bit)2]·H2O, is itself prepared in high yields upon reaction of Na[bit] with Na2[PdCl4] in methanol and the analogous platinum complex, [Pt(bit)2]·H2O, is similarly prepared from K2[PtCl4]. It is not clear if these species are mono- or dimeric, and formulation as [M2(μ-bit)4(H2O)2] with the four benzisothiazolinate spanning the metal-metal vector and possibly binding through coordination of nitrogen and oxygen is suggested. Diphosphine adducts, cis-[Pd(bit)2{κ2-Ph2P(CH2)nPPh2}] (n = 1-4) can be prepared both upon addition of the diphosphine to [Pd(bit)2]·H2O and from reactions of cis-[PdCl2{κ2-Ph2P(CH2)nPPh2}] with two equivalents of Na[bit]. A crystal structure of cis-[Pd(bit)2(κ2-dppe)] reveals that the benzisothiazolinate ligands are bonded in a monodentate fashion through nitrogen and this binding mode is proposed for all [Pd(bit)2L2] and [Pd(bit)2L] complexes. With dppb (n = 4) a second product is seen by NMR spectroscopy being proposed to be the part-substituted complex cis-[PdCl(bit)(κ2-dppb)], while with dppm (n = 1) two further products are seen spectroscopically, proposed as trans-[Pd(bit)2(κ1-dppm)2] and (more tenuously) [Pd2(bit)4(dppm)2]. The former is also prepared in good yields from reaction of [Pd(κ2-dppm)2]Cl2 with Na[bit]. These studies show that palladium benzisothiazolinate are easily accessed and show good air and moisture stability.
- Al-Jibori, Subhi A.,Ahmed, Birgul S.M.,Ahmed, Safaa A.,Karada?, Ahmet,Schmidt, Harry,Wagner, Christoph,Hogarth, Graeme
-
-
Read Online
- Synthesis and bioactivity of novel 2-(1,2-benzisothiazol-3-yloxy)-N-(1-aryl-3-cyanopyrazol-5-yl) acetamides
-
Nine novel types of 2-(1,2-benzisothiazol-3-yloxy)-N-(1-aryl-3-cyanopyrazol-5-yl)-acetamides were synthesized, and their inhibition effects on selected bacteria (heterotrophic bacteria) and algae (marine chlorella) were evaluated. Results showed that 2-(1,2-benzisothiazol-3-yloxy)-N-(3-cyano-1-(2,4-dimethylphenyl)pyrazol-5-yl) acetamide achieved the highest yield of 81% with good bioactivity against heterotrophic bacteria and marine chlorella.
- Yu, Peng,Li, Xi,Zhang, Xiao,Xu, Yanhua
-
p. 397 - 405
(2020/09/04)
-
- 2-butyl-1,2-benzisothiazolin-3-one preparation method
-
The present invention discloses a 2-butyl-1,2-benzisothiazolin-3-one synthesis process, which comprises that (1) a starting raw material BIT reacts with an alkali to form a BIT salt; and (2) the BIT salt reacts with halogenated n-butane to obtain the target product 2-butyl-1,2-benzisothiazolin-3-one (BBIT). The present invention further discloses a separation and purification method of 2-butyl-1,2-benzisothiazolin-3-one, wherein an acid is added to a mixture containing BBIT to make the BBIT form the salt, and the obtained BBIT salt is alkalized so as to obtain the high purity BBIT. According to the present invention, the synthesis method has advantages of easily available raw materials, mild reaction condition, high yield, low cost, low environmental pollution and convenient industrial production; and with the separation and purification method, the high purity target product can be obtained, and the method can be widely used for industrial production.
- -
-
Paragraph 0055-0056
(2017/09/08)
-
- Process for preparing benzisothiazolinones
-
N-alkylated 1,2-benzisothiazolin-3-ones can be prepared in good yield and good selectivity by reaction of the lithium salt of 1,2-benzisothiazolin-3-one with an electrophilic alkylating agent.
- -
-
Paragraph 0019
(2014/11/27)
-