Synthesis and application of nitrosourea compounds modified by benzisoselenazocone
A technology of benzisoselenazole and compounds, which is applied in the field of preparation of nitrosourea compounds modified by benzisoselenazole, can solve problems such as pulmonary fibrosis
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Embodiment 1
[0082] Embodiment 1 2, the preparation of 2'-diselenide bisbenzoic acid
[0083] 2Se+4NaOH+Na 2 S 2 o 4 →Na 2 Se 2 +2Na 2 SO 3 +2H 2 o
[0084]
[0085] (1) 16g of sodium hydroxide, 18g of sodium hydrosulfite, and 16g of selenium powder were added into water successively, and the temperature was raised to 50° C., and the reaction was completed to obtain a sodium diselenide solution.
[0086] (2) Under ice-bath conditions, 28 g of anthranilic acid was added to 80 ml of 1:1 hydrochloric acid and stirred and mixed, and an aqueous solution of 18.0 g of sodium nitrite was slowly added dropwise therein to obtain 2-benzoic acid diazonium chloride.
[0087] (3) Add the solution of 2-benzoic acid diazonium chloride obtained in step 1 dropwise into the sodium diselenide solution obtained in step 2 under stirring in an ice-water bath, and the mixture continues to stir. pH paper proves that the solution is alkaline. Filter with celite, adjust the pH to 3, filter, wash the fil...
Embodiment 2
[0089] The preparation of embodiment 2 2-selenium chlorobenzoyl chlorides
[0090]
[0091] 40g of 2,2'-diselenide bisbenzoic acid, 200ml of thionyl chloride and a few drops of DMF were stirred and refluxed. After the reaction was completed, excess thionyl chloride was removed by rotary evaporation, and the residue was recrystallized with petroleum ether to obtain yellow needle-like crystals.
[0092] 1 H NMR (400MHz, CDCl 3): δδ7.39(t, J=7.7Hz, 1H, Ar-H), 7.67(t, J=7.7Hz, 1H, Ar-H), 7.85(d, J=7.7Hz, 1H, Ar-H ), 8.09 (d, J=7.7Hz, 1H, Ar-H).
Embodiment 3
[0093] Example 3 Preparation of 5,5'-difluoro-2,2'-diselenide bisbenzoic acid
[0094] 2Se+4NaOH+Na 2 S 2 o 4 →Na 2 Se 2 +2Na 2 SO 3 +2H 2 o
[0095]
[0096] This compound was obtained in the same manner as in Example 1.
[0097] 1 H NMR (400MHz, DMSO-d 6 ): δδ7.23(m, 2H), 7.40(dd, 2H), 8.11(m, 2H), 13.93(s, br, 2H)
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