Reduction of certain 2,2{40 -disubstituted azoxybenzenes and azobenzenes to corresponding hydrazobenzenes
阅读：17发布：2022-10-03
专利汇可以提供Reduction of certain 2,2{40 -disubstituted azoxybenzenes and azobenzenes to corresponding hydrazobenzenes专利检索，专利查询，专利分析的服务。并且Certain 2,2''-disubstituted hydrazobenzenes, including 2,2''dichlorohydrazobenzene, 2,2''-dimethylhydrazobenzene, and 2,2''dimethoxyhydrazobenzene are produced from the corresponding 2,2''azoxy or azobenzene by a variation of the classical Bechamp reaction for the preparation of anilines, using iron filings and dilute acid. The reaction is accelerated by the employment of small amounts of lead as a reaction promoter and by employment of a solvent and preferably also a cosolvent. When applied to the preferred 2,2''-dichloro starting materials, the reaction is especially valuable in that it produces exceptionally high yields and purity of desired product with a minimum of amine and other byproducts.，下面是Reduction of certain 2,2{40 -disubstituted azoxybenzenes and azobenzenes to corresponding hydrazobenzenes专利的具体信息内容。
1. A METHOD FOR THE PRODUCTION OF A 2,2''-DISBSTITUTED HYDRAZOBENZENE, SELECTED FROM THE GROUP CONSISTING OF 2,2''DICHLOROHYDRAZOBENZENE, 2,2''-DIMETHYLHYDRAZOBENZENE, AND 2,2'' -DIMETHOXYHYDRAZOBENZENE, BY THE REDUCTION OF A COMPOUND SELECTED FROM THE GROUP CONSISTING OF 2,2 DICHLOROAZOXYBENZENE, 2,2''-DICHLOROAZOBENZENE, 2,2'' -DIMETHYLAZOXYBENZENE, 2,2''-DICHLOROAZOBENZENE, 2,2'' -DIMETHOXYAZOXYBENZENE, AND 2,2'' -DIMETHOXYAZOBENZENE, COMPRISING THE STEP OF EFFECTING THE REDUCTION OF THE STARTING DISUBSTITUTED AZOXYBENZENE OR DISUBSTITUTED AZOBENZENE WITH FINELY-DIVIDED IRON AND DILUTE ACID.
2. A method of claim 1 wherein at least about the stoichiometric amount of iron is employed.
3. A method of claim 1 wherein reaction is conducted in the presence of lead as a reaction accelerator.
4. The method of claim 3 wherein the lead is added to the reaction mixture as a lead salt.
5. A method of claim 3 wherein the lead is deposited on the iron and the coated iron employed in the reaction.
6. A method of claim 1 wherein the starting material is 2,2''-dichloroazoxybenzene and the product is 2,2''-dichlorohydrazobenzene.
7. A method of claim 1 wherein the starting material is 2,2''-dichloroazobenzene and the product is 2,2''-dichlorohydrazobenzene.
8. A method of claim 1 wherein the reaction is conducted in the presence of a water-immiscible organic solvent for the starting azoxy or azobenzene, which solvent is non-reactive with the reactants and reaction products under the conditions of reaction.
9. A method of claim 8 wherein the solvent employed is an aromatic hydrocarbon solvent.
10. A method of claim 9 wherein the solvent employed is benzene, toluene, or xylene.
11. A method of claim 8 wherein the reaction is conducted in the presence of a cosolvent.
12. A method of claim 11 wherein the cosolvent is a lower-alkanol.
13. A method of claim 11 wherein the cosolvent is methanol.
14. A method of claim 1 wherein the reaction is conducted at a temperature between about 45* and about 75* C.
15. A method of claim 1 wherein the reaction is conducted at a temperature between about 55* and about 65* C.
16. A method of claim 1 wherein the acid is employed in an amount up to about the stoichiometric amount.
17. A method according to claim 1 wherein the acid is employed in an amount less than the stoichiometric amount.
18. A method of claim 1 wherein the acid employed is a mineral acid.
19. A method of claim 1 wherein the acid employed is hydrochloric acid.
20. A method of claim 18 wherein the acid is employed in a concentration up to about 7.3% by weight.
21. A method of claim 3 wherein the lead is employed in an amount up to about 5% by weight of the iron.
22. A method of claim 3 wherein the lead is employed in an amount up to about one percent by weight of the iron.
23. A method of claim 1 wherein the starting material is 2,2''-dichloroazoxybenzene, the acid is hydrochloric acid in a concentration of up to about 7.3% by weight and in an amount not substantially greater than the stoichiometric amount, and wherein the reaction is carried out at a temperature up to about 75* C. in the presence of a water-immiscible organic solvent.
24. A method of claim 23 wherein the water-immiscible organic solvent is an aromatic hydrocarbon.
25. A method of claim 23 wherein the reaction is conducted in the presence of lead in an amount up to about one percent by weight of the iron.
26. A method of claim 23 wherein a lower-alkanol cosolvent is also present.
27. A method of claim 25 wherein methanol is present as cosolvent.
28. A method of claim 23 wherein the reaction is conducted at a temperature between about 55* and about 65* C.
29. In a process for the iron-acid reduction of a reduced nitrobenzene in which the final reduction stage involves a fission of the produced hydrazobenzene into two molecules of the corresponding aniline, the improvement in which the starting compound is a 2,2''-disubstituted azoxy- or azobenzene selected from the group consisting of 2,2''-dichloroazoxybenzene, 2,2''-dichloroazobenzene, 2,2''-dimethylazoxybenzene, 2,2''-dimethylazobenzene, 2,2''-dimethoxyazoxybenzene, and 2,2''-dimethoxyazobenzene, said process being uniquely characterized in that the reduction does not go substantially beyond the hydrazobenzene stage, whereby the predominant product is a 2,2''-disubstituted hydrazobenzene selected from the group consisting of 2,2''-dichlorohYdrazobenzene, 2,2''-dimethylhydroazobenzene, and 2,2''-dimethoxyhydrazobenzene.
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