2, 3-dichloro-5-(trifluoromethyl)pyridine (DCTF) yog ib qho tseem ceeb organic intermediate rau kev lag luam agrochemical tshwj xeeb rau kev siv nyob rau hauv cov synthesis ntawm fluazinam thiab fluopicolide nrog rau lwm yam tshuaj tua kab active pyridine tebchaw.
Txheej txheem cej luam ntawm Synthetic Routes
1) Siv 2,3-dichloro-5-trichloromethylpyridine ua raw khoom
106.16 g (0.4 mol) ntawm 2, 3-dichloro-5-trichloromethylpyridine thiab 180 g (9 mol) ntawm anhydrous hydrogen fluoride tau muab ntxiv rau hauv lub tshuab hluav taws xob polyethylene, thiab tswj qhov kub thiab txias. ntawm -20 degree nyob rau hauv 3 h Maj mam ntxiv mercuric oxide, tswj cov tshuaj tiv thaiv kub ntawm lub cev tsis pub tshaj 35 degree , thiab do cov tshuaj tiv thaiv rau li 22 teev tom qab ntxiv, kom txog thaum lub kaw lus yog grey-dawb. Lim, neutralize lub filtrate nrog sodium bicarbonate, extract nrog dichloromethane, qhuav nrog anhydrous sodium sulfate, tshem tawm cov dichloromethane nyob rau hauv lub siab txo kom tau cov khoom 2, 3-dichloro-5-trifluoromethylpyridine, tus nqi conversion yog 100%. , thiab kev xaiv yog 98%.
2) Siv 3-methylpyridine ua raw khoom
Noj 50 g ntawm 2, 3-dichloro-5-trichloromethylpyridine, ntxiv catalyst, kub txog 170 degree, maj mam qhia cov pa roj hydrogen fluoride, thiab ua rau 11 teev. Tom qab cov tshuaj tiv thaiv tiav lawm, siv 5% sodium bicarbonate tov nyob rau hauv Thiab, cov organic theem tau sib cais, ntxuav nrog dej, thiab qhuav kom tau ib tug crude khoom nrog ib tug cov ntsiab lus ntawm 85% thiab yield ntawm 65%.
3) Siv 2-chloro-5-trifluoromethylpyridine ua raw khoom
Noj 363 g ntawm 2-chloro-5-trifluoromethylpyridine, ntxiv 325 g ntawm ferric chloride, dhau cov roj chlorine, cua sov mus rau 150-170 degree thiab ua rau 18 h, ntxiv cov tshuaj tiv thaiv rau 1.5 L. dej kub, cais tawm Cov roj txheej tau qhuav nrog anhydrous sodium sulfate thiab rectified kom tau 163 g ntawm cov khoom.