Method for synthesizing plasticizer 3-nitro furazan-4-methyl ether
A technology of nitrofurazan and synthesis method, which is applied in the synthesis of plasticizer 3-nitrofurazan-4-methyl ether, and in the field of plasticizer synthesis, which can solve problems such as delayed detonation
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[0007] The raw materials ethyl cyanoacetate, hydroxylamine hydrochloride, sodium nitrite, sodium hydroxide, sodium borohydride, zinc chloride, concentrated sulfuric acid, hydrogen peroxide, thionyl chloride, pyridine, sodium methoxide, acetonitrile etc. used in the present invention are analysis Pure reagents.
[0008] (1) Synthesis of AFCA
[0009] Take 138g (2mol) sodium nitrite and 1600ml distilled water to make a solution, 226.4g (2mol) ethyl cyanoacetate and 140ml EtOH to make a solution, pour it into a 2L flask. Take 80ml85%H 3 PO 4 Add dropwise and stir at room temperature for 1h. Lower to 10°C and stir overnight. Add 16Og (4mol) NaOH, 278g (4mol) NH 2 OH·HCI and 336 g (6 mol) KOH, stirred for 1 h. Heated to reflux for 2h. Cool in an ice bath to ambient temperature and adjust the pH to 6 with concentrated hydrochloric acid, and filter off the white solid. Continue to adjust the pH until a white solid precipitates, filter with suction, and recrystallize the filte...
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