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Kev lis kev cai code: 2942000000
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Daim ntawv thov
Organic hluavtaws intermediate, ib tug sterically hindered, non-nucleophilic puag uas txawv ntawm Brnsted (protonic) thiab Lewis acids.Ua kom qhov ncaj qha high-yield conversion ntawm aldehydes1 thiab ketones1,2 rau vinyl triflates.
2,6-Di-tert-butyl-4-methylpyridine yog ib qho organic compound nrog molecular mis C14H23N, ib qho tseem ceeb nruab nrab ntawm cov organic synthesis, feem ntau yog siv nyob rau hauv kws intermediates, organic synthesis, organic solvents, kuj yuav siv tau nyob rau hauv dye ntau lawm, tshuaj tua kab. ntau lawm thiab fragrances, thiab lwm yam.
Txoj kev tsim khoom
1. Ua 2,6 di-tert-butyl-4-methylbenzyl trifluoromethanesulfonate Nyob rau hauv ib lub 100-mL triple flask nruab nrog ib tug nitrogen qhia raj, ib tug tas li siab funnel, ib tug electromagnetic stirring bar thiab ib tug ice condenser nrog ib tug qhuav raj, ntxiv 24.2 g (0.2 mol) ntawm trimethylethyl phthalide chloride thiab 3.7 g (0.05 mol) ntawm tert-butanol.Cov tshuaj tiv thaiv sib tov tau rhuab hauv ib lub roj da dej rau 85 ° C.Tom qab ntawd 15 g (0.1 mol) ntawm trifluoromethanesulfonic acid ntxiv rau ntau tshaj 15 feeb.Cov tshuaj tiv thaiv tau txuas ntxiv rau 10 feeb, thiab cov khoom siv tshuaj tiv thaiv xim av tau txias rau hauv ib da dej dej khov thiab nchuav rau hauv 100 ml ntawm ether txias.Cov xim av precipitate tau lim thiab qhuav kom tau 9.6 g (54%) ntawm qeeb buzz ntsev.(Tsis muaj purification yog yuav tsum tau: rau cov kauj ruam tom ntej ntawm kev npaj, recrystallize ob zaug ntawm chloroform mus rau carbon tetrachloride 3: 1) mus rau xim tsis muaj koob zoo li crystals.
2. Kev npaj ntawm 2,6-Di-tert-butyl-4-methyl-vizine Nyob rau hauv stirring, ib tug ncua kev kawm ntawv ntawm 10 g (0.028 mol) ntawm crude ntsev ntawm vizine nyob rau hauv 200 mL ntawm 95% ethanol chilled mus rau 60 ° C yog Ntxiv ib zaug mus rau 100 mL ntawm concentrated ammonia chilled rau 60 ° C nyob rau hauv 1-liter vaj-hauv qab hwj.Cov tshuaj tiv thaiv tau txuas ntxiv ntawm 60 ° C rau 30 feeb thiab 40 ° C rau 2 teev, thaum lub sijhawm ncua kev tshem tawm.Tom qab ntawd, cov tshuaj tiv thaiv sib tov yog nchuav rau hauv 500 ml ntawm 2% sodium hydroxide tov maj mam sov rau hauv chav sov.Extracted nrog .4-100 ml ntawm pentane, ua ke rho tawm, 25 ml ntawm saturated sodium chloride tov ntxuav, 100 ml ntawm pentane teb evaporator concentration.