Synthesis txoj kev ntawm 4-aminoantipyrine

1. Antipyrine yog nitrosated los ntawm sodium nitrite, txo los ntawm ammonium bisulfite thiab ammonium sulfite, hydrolyzed los ntawm sulfuric acid, thiab thaum kawg neutralized nrog kua ammonia kom tau 4-aminoantipyrine. Cov txheej txheem yog raws li nram no: Antipyrine yog tov nrog 50% sulfuric acid los tsim ib tug tov, uas muaj 38% -40% antipyrine thiab 11% -12% sulfuric acid. Cov tshuaj no thiab sodium nitrite tov tau ntws mus rau hauv nitrosation reactor tib lub sij hawm, qhov ntws ntawm ob yog tswj, cov tshuaj tiv thaiv kub ntawm 45-50 ° C, cov tshuaj tiv thaiv yog nplawm, thiab qhov kawg taw tes ntawm cov tshuaj tiv thaiv yog. ntsuas nrog iodine hmoov starch test ntawv los kho cov dej ntws. Nitroso-antipyrine generated los ntawm nitrosation tam sim ntawd ntws mus rau hauv lub tank txo thiab reacts nrog aqueous tov ntawm ammonium bisulfite thiab ammonium sulfite, uas yog ib tug txo tus neeg sawv cev npaj nyob rau hauv lub tank. Siv ib qho piv txwv los ntsuas pH tus nqi thiab qib ntawm kev txo qis. Tus nqi pH yog nyob nruab nrab ntawm 5.4 thiab 5.8, thiab qib ntawm kev txo qis yog li 15 (uas yog, 1ml ntawm kev txo cov tshuaj noj cov milliliters ntawm 0.1N iodine tov). Tom qab qhov txo qis, tus nqi pH raug hloov mus rau 5. Txias mus rau 80 ° C, neutralize rau pH 7-7.5 nrog kua ammonia, thiab sawv ntsug rau stratification. Cais cov dej khib nyiab kom tau 4-aminoantipyrine roj (siab dua 80% cov ntsiab lus). Nias nws rau hauv lub tank crystallization, do, txias kom crystallize, thiab lim kom tau 4-aminoantipyrine.

2. Antipyrine yog nitrosated, ces txo los ntawm ammonium bisulfite thiab ammonium sulfite, hydrolyzed nrog sulfuric acid, thiab thaum kawg neutralized nrog kua ammonia kom tau 4-amino antipyrine.