Preparation method of N-(carboxymethyl aminocarbonyl)-4, 4 '-bis (dimethylamino) diphenylamine sodium salt
A technology of nitrosodimethylaniline hydrochloride and carboxymethylamino is applied in the field of preparation of N--4,4'-bis-diphenylamine sodium salt, which can solve the problem of unretrievable and unfavorable reduction of glycosylated hemoglobin In order to reduce production costs and improve production efficiency
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Embodiment 1
[0064] N-(carboxymethylaminocarbonyl)-4,4'-bis(dimethylamino)diphenylamine sodium salt I, its molecular formula is C 19 H 23 N 4 NaO 3 , the molecular weight is 378.40069, and the structural formula is shown in I.
[0065]
[0066] Following is the preparation method of N-(carboxymethylaminocarbonyl)-4,4'-bis(dimethylamino)diphenylamine sodium salt I:
[0067] S1. N,N-dimethylaniline shown in formula II reacts with sodium nitrite and hydrochloric acid to obtain p-nitrosoxylidine hydrochloride shown in formula III;
[0068] in,
[0069] S11. Take a 1L dry three-necked flask, add 1mol of N,N-dimethylaniline shown in formula II and 420ml of hydrochloric acid solution containing chloride ions into the three-necked flask in turn, mix and stir evenly, the reaction solution gradually turns pink To clarify the solution, cool down the three-necked flask to ensure that the internal temperature of the three-necked flask is 0°C. At this time, drop solution a into the bottle. Solut...
Embodiment 2-6
[0120] The preparation methods of Examples 2-6 are the same as those of Example 1, and the difference is only that the amount of substances added in each step is different, and thus the final yield of each step will also be different.
[0121] In conjunction with embodiment 1, the difference data of this part are specifically shown in table 1 to table 6:
[0122] Table 1 The addition amount of each chemical substance and the yield of substance III in step S1
[0123]
[0124] Table 2 The addition amount of each chemical substance and the yield of substance IV in step S2
[0125]
[0126] Table 3 The addition amount of each chemical substance and the yield of substance V in step S3
[0127]
[0128] Table 4 The addition amount of each chemical substance and the yield of substance VII in step S4
[0129]
[0130] The addition amount of each chemical substance and the yield of substance IX in step S5 of table 5
[0131]
[0132] Table 6 The addition amount of ea...
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