- Method for preparing 1,1,1,3,3-pentachlorobutane
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The invention discloses a method for preparing 1,1,1,3,3-pentachlorobutane. According to the method, carbon tetrachloride and 2-chloropropene have a telomerization reaction through a telomerization catalyst to prepare 1,1,1,3,3-pentachlorobutane, wherein the reaction temperature ranges from 25 DEG C to 100 DEG C, and the reaction time ranges from 0.5 h to 5 h. The telomerization catalyst is prepared from a main catalyst, an auxiliary catalyst and an organic active agent, wherein halogenated copper salt or halogenated iron salt serves as the main catalyst, alkyl phosphate or diisopropyl phosphate or organic tertiary amine serves as the auxiliary catalyst, azodiisobutyronitrile, 2,2-azobis(4-methoxy-2,4-dimethylvaleronitrile), 1,1-azo-Biscyclohexanecarbonitrile, ascorbic acid, 2,3,4,5,6-5-hydroxy aldehyde, phenylhydrazine or metoxyphenol serves as the organic active agent, and the molar ratio of the main catalyst to the auxiliary catalyst to the organic active agent is 1:(0.5-20):(0.1-20). The telomerization catalyst has the advantages of being mild in reaction conditions and stable in air and can be used for catalyzing the telomerization reaction between carbon tetrachloride and 2-chloropropene to prepare 1,1,1,3,3-pentachlorobutane.
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Paragraph 0028; 0029; 0040
(2016/12/01)
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- PROCESS FOR PREPARATION OF 1,1,1,3,3-PENTACHLOROBUTANE
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A process for preparation of 1,1,1,3,3-pentachlorobutane comprises reacting carbon tetrachloride and 2-chloropropene, in which the catalyst includes main catalyst and co-catalyst. The said main catalyst is one or more catalysts selected from the group consisting of Fe (II) salt, Fe or Fe (III) salt, co-catalyst is one or more catalysts selected from the group consisting of alkyl phosphites, alkyl phosphates or aryl phosphates. The said process has high yield and selectivity, and the catalyst is conveniently separated from the product.
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Page/Page column 4
(2009/08/14)
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- PROCESS FOR THE PREPARATION OF HALOGENATED HYDROCARBONS WITH AT LEAST 3 CARBON ATOMS
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A telomerisation process is described wherein a halocarbon is added to olefins like 2-chloroprop-1-ene in the presence of ionic liquids and/or compounds having at least two nitrogen atoms at least one of which is tricordinated and at least one of which is tetracoordinated. The reaction products, e.g. 1,1,3,3-tetrachloro-1-fluorobutane, can be further fluorinated.
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Page/Page column 16
(2008/06/13)
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- PROCESS FOR THE PREPARATION OF HALOGENATED HYDROCARBONS WITH AT LEAST 3 CARBON ATOMS IN THE PRESENCE OF A RUTHENIUM COMPOUND
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A telomerisation process is described whereby haloalkanes like tetrachloromethane are added to halogensubstituted olefins like 2-chloroprop-1- ene in the presence of a Ru catalyst. The reaction products, e.g. 1,1,1,3,3-pentachlorobutane, can be fluorinated.
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Page/Page column 6
(2008/06/13)
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- Process for the preparation of halogenated hydrocarbons with at least 3 carbon atoms in the presence of Iron and a phosphite
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A telomerisation process is described whereby haloalkanes like tetrachloromethane are added to halogenated olefins like 2-chloroprop-1-ene in the presence of an iron catalyst and a phosphite. The reaction products, e.g. 1,1,1,3,3-pentachlorobutane, can be fluorinated.
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Page/Page column 3
(2008/06/13)
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- Process for preparing halohydrocarbons
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Halohydrocarbons containing at least 3 carbon atoms are obtained by reaction between a haloalkane and an olefin in the presence of a catalyst in a reaction medium which is essentially free of water.
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Page column 4, 5
(2008/06/13)
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- Carbonyl ylides and carbenes from thermolysis of oxadiazolines. Substituent effects on intramolecular and intermolecular reactions of carbonyl ylides
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Thermolysis of a 2-methoxy-Δ3-1,3,4-oxadiazoline involves loss of N2 with formation of carbonyl ylide.The fate of the carbonyl ylide depends on its enviroment and on the other substituents present.Thus, the ylides from 2-methoxy-2,5,5-trimethyl-Δ3-1,3,4-oxadiazoline (1) and from 2-methoxy-2-(4-methoxyphenyl)-5,5-dimethyl-Δ3-1,3,4-oxadiazoline (2) are trapped very efficiently by methanol.However, the ylide from 1 is trapped much less efficiently than that from 2 by dimethylacetylene dicarboxylate, cis-1,2-dichloroethylene, or norbornadiene.A major competitive process in the case of 1 is fragmentation of the ylide to carbonyl compounds and carbenes, the latter being trapped by alkenes to form cyclopropanes.An intramolecular 1,4-H transfer is also competitive under some conditions.The ylide from 2 does not appear to fragment, nor does it undergo the 1,4-H transfer, but it cyclizes efficiently to the oxirane in the absence of trapping agents.Preliminary estimates of rate constants for cyclization of ylide from 2 to form the oxirane (kcycl31 deg C = 1.3*1E-6 s-1) and for its additions to norbornadiene and to dimethylacetylene dicarboxylate (1*1E-5 M-1s-1 and 1*1E-9 M-1s-1, respectively are reported.If it is assumed that the ylide from 1 would add to dimethylacetylene dicarboxylate with a similar rate constant, then the yield for that process can be used to place a lower limit of 1010s-1 on the rate constant for fragmentation of that ylide at 31 deg C.
- Bekhazi, Michel,Warkentin, John
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p. 619 - 624
(2007/10/02)
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