Polychlorinated metallocenes and their synthesis
阅读：754发布：2022-06-23
专利汇可以提供Polychlorinated metallocenes and their synthesis专利检索，专利查询，专利分析的服务。并且Novel polychlorinated metallocenes are provided that have the following formulas: C5H5 mClmMC5H5 and (C5H5 nCln)2M, wherein M is iron, ruthenium or osmium, m is an integer from 3 to 5, inclusive, and n is an integer from 2 to 5, inclusive. The products are prepared by (1) reacting a monochlorometallocene or a 1,1''-dichlorometallocene with an organolithium compound in the presence of a solvent, (2) recovering a 1-chloro-2lithiometallocene or a 1,1''-dichloro-2,2''-dilithiometallocene depending upon the starting material used, and (3) then reacting one of the latter compounds with a chlorination agent to obtain 1,2-dichlorometallocene or 1,1'',2,2''-tetrachlorometallocene. The lithiation step and the chlorination step can then be repeated one, two, 3 or more times, using in each reaction as the starting material the isolated chlorinated product from the prior reaction. The polychlorinated metallocenes are useful in preparing metallocene-containing polymers that are particularly suitable as ablative plastics for heat shields and structural laminates for light weight radiation shields. They also can be used to synthesize high temperature and/or high density fluids as well as for additives for lubricants and as flame retardant additives. The decachlorometallocenes are particularly useful because of their high resistance to oxidation.，下面是Polychlorinated metallocenes and their synthesis专利的具体信息内容。
2. adding a chlorinating agent to the resulting reaction mixture; and recovering a reaction mixture containing a 1,1'' , 2,2''-tetrachlorometallocene when the chlorinated metallocene selected is a dichlorometallocene or a 1,2-dichlorometallocene when the chlorinated metallocene selected is a chloro-metallocene.
2. adding a chlorinating agent to the resulting reaction mixture;
2. adding a chlorinating agent to the resulting reaction mixture;
2. A composition according to claim 1 in which a polychlorinated metallocene has the structure of Formula (1) in which M is iron and R1, R2, R3, and R4 are each Cl.
3. A composition according to claim 1, in which a polychlorinated metallocene has the structure of Formula (1) in which M is ruthenium and R1, R2, R3, and R4 are each Cl.
3. recovering a first reaction mixture containing chlorinated ruthenocenes;
3. recovering a first reaCtion mixture containing chlorinated ferrocenes;
4. separating said chlorinated ferrocenes from said first reaction mixture;
4. separating said chlorinated ruthenocenes from said first reaction mixture;
4. A composition according to claim 1 in which a polychlorinated metallocene has the structure of Formula (1) in which M is iron, R1 is I and R2, R3 and R4 are each Cl.
5. A composition according to claim 1 in which a polychlorinated metallocene has the structure of Formula (1) in which M is iron, R1 is L; and R2, R3and R4 are each Cl.
5. reacting said chlorinated ruthenocenes with said organolithium in the presence of said solvent;
5. reacting said chlorinated ferrocenes with said organolithium compound in the presence of said solvent;
6. adding a chlorinating agent to the resulting reaction mixture;
6. adding a chlorinating agent to the resulting reaction mixture;
6. A composition according to claim 1 in which a polychlorinated metallocene has the structure of Formula (1) in which M is iron, R1 is COOH and R2, R3 and R4 are each Cl.
7. A composition according to claim 1 in which a polychlorinated metallocene has the structure of Formula (2) in which M is iron and R3 and R4 are each Cl.
7. recovering a second reaction mixture containing chlorinated ruthenocenes;
7. recovering a second reaction mixture containing chlorinated ferrocenes;
8. repeating steps (4), (5), (6), (7), and (8) in succession three additional times, using respectively, as a starting material said second and a third and a fourth reaction mixture containing chlorinated ferrocenes;
8. repeating steps (4), (5), (6) and (7) in succession four additional times, using, respectively, as a starting material said second and a third, a fourth and a fifth reaction mixture, each containing chlorinated ruthenocenes;
8. A process for preparing a polychlorinated metallocene which comprises the follOwing steps:
9. recovering a sixth reaction mixture containing chlorinated ruthenocenes; and
9. recovering a fifth reaction mixture containing chlorinated ferrocenes; and
9. The process according to claim 8 in which a 1,1'' ,2,2''-tetrachlorometallocene or a 1,2-dichlorometallocene is separated from said reaction mixture; said 1,1'',2,2''-tetrachlorometallocene or said 1,2-dichlorometallocene is reacted with said organolithium compound; a chlorinating agent is added to the resulting reaction mixture; and a second reaction mixture is recovered containing a 1,1'' ,2,2'', 3,3''-hexachlorometallocene when a 1,1'' ,2,2''-tetrachlorometallocene is a reactant or a 1,2, 3,-trichlorometallocene when a 1,2-dichlorometallocene is a reactant.
10. The process according to claim 9 in which a 1,1'' ,2,2'' ,3, 3''-hexachlorometallocene or a 1,2,3-trichlorometallocene is separated from said second reaction mixture; said 1,1'' ,2,2'' ,3, 3''-hexachlorometallocene or said 1,2,3-trichlorometallocene is reacted with said organolithium compound; a chlorinating agent is added to the resulting reaction mixture; and a third reaction mixture is recovered containing a 1,1'' ,2,2'' ,3,3'' ,4,''-octachlorometallocene when a 1,1'' ,2,2'' ,3,3''-hexachlorometallocene is a reactant or a 1,2,3,4-tetrachlorometallocene when a 1,2,3-trichlorometallocene is a reactant.
10. separating decachloroferrocene from said fifth reaction mixture.
10. separating decachlororuthenocene from said sixth reaction mixture.
11. The process according to claim 10 in which a 1,1'' ,2,2'' ,3, 3'' ,4,4''-octachlorometallocene or a 1,2,3,4-tetrachloro-metallocene is separated from said third reaction mixture; said 1,1'' ,2,2'' ,3,3'' 4,4''-octachlorometallocene or said 1,2,3,4-tetrachlorometallocene is reacted with said organolithium compound; a chlorinating agent is added to the resulting reaction mixture, and a fourth reaction mixture is recovered containing a 1,1'' ,2,2'' 3,3'' ,4,4'' ,5,5''-decachlorometallocene when a 1,1'' ,2, 2'' ,3,3'' ,4,4''-octachlorometallocene is a reactant or a 1,2,3,4, 5-pentachlorometallocene when a 1,2,3,4-tetrachlorometallocene is a reactant.
12. The process according to claim 11 in which said fourth reaction mixture contains 1,1'' ,2,2'' ,3,3'' ,4,4'' ,5,5''-decachloroferrocene.
13. The process according to claim 11 in which said fourth reaction mixture contains 1,1'' ,2,2'',3,3'' 4,4'' ,4,4''-decachlorouthenocene.
14. The process according to claim 11 in which said fourth reaction mixture contains 1,2,3,4,5-pentachloroferrocene.
15. The process according to claim 8 in which said chlorinated metallocene is reacted in step (1) with a complex of said organolithium compound and an aliphatic diamine.
16. The process according to claim 15 in which said organolithium compound is n-butyllithium and said aliphatic diamine is N,N,N'' ,N''-tetramethylethylenediamine.
17. A process for preparing 1,1'' ,2,2'' ,3,3'' ,4,4'' ,5,5''-decachloroferrocene which comprises the following steps:
18. A process according to claim 17 in which said organolithium compound is n-butyllithium and said chlorinating agent is hexachloroethane.
19. A process according to claim 17 in which lithiation step (1) and chlorination step (2) and all subsequent lithiation and chlorination steps except the last lithiation and chlorination steps are conducted at a temperature in the range of about 0* to 40* C., and the last lithiation and chlorination steps are conducted at a temperature in the range of about -5* to 5* C.
20. A process for preparing 1,1'' ,2,2'' ,3,3'' ,4,4'' ,5,5''-decachlororuthenocene which comprises the following steps:
21. A process according to claim 20 in which said organolithium compound is n-butyllithium and said chlorinating agent is hexachloroethane.
22. A process according to claim 20 in which lithiation step (1) and chlorination step (2) and all subsequent lithiation and chlorination steps except the last lithiation and chlorination steps are conducted at a temperature in the range of about 0* to 40* C., and the last lithiation and chlorination steps are conducted at a temperature in the range of about -5* to 5* C.
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