CAJ | 학술논문

实验以对乙酰氨基酚和三氯硫磷为原料,经酯化反应合成硫代磷酸三(4-乙酰氨基苯)酯(TPTAA),讨论了反应介质、缚酸剂种类、对乙酰氨基酚与三氯硫磷的物质的量的配比、缚酸剂用量与组成等因素对TPTAA产率的影响,结果表明:在n(对乙酰氨基酚):n(三乙胺+吡啶):n(三氯硫磷)=3.10:3.80:1、n(三乙胺):n(吡啶)=1:0.02、反应温度35℃、反应时间4 h条件下,TPTAA的收率可达到88.04%;再将TPTAA在酸性条件下水解得到硫代磷酸三(4-氨基苯)酯(TPTA),探讨了HCl和CH_3OH用量对产物产率的影响,得到:当n(CH_3OH):n(HCl):n(TPTAA)=2.9:6.0:1,反应温度85℃,反应时间3 h时,TPTA的收率95.62%.
실험이대을선안기분화삼록류린위원료,경지화반응합성류대린산삼(4-을선안기분)지(TPTAA),토론료반응개질、박산제충류、대을선안기분여삼록류린적물질적량적배비、박산제용량여조성등인소대TPTAA산솔적영향,결과표명:재n(대을선안기분):n(삼을알+필정):n(삼록류린)=3.10:3.80:1、n(삼을알):n(필정)=1:0.02、반응온도35℃、반응시간4 h조건하,TPTAA적수솔가체도88.04%;재장TPTAA재산성조건하수해득도류대린산삼(4-안기분)지(TPTA),탐토료HCl화CH_3OH용량대산물산솔적영향,득도:당n(CH_3OH):n(HCl):n(TPTAA)=2.9:6.0:1,반응온도85℃,반응시간3 h시,TPTA적수솔95.62%.
Tris(4-acetamindophenyl)thiophosphate(TPTAA)was synthesized using P-acetoamidophenol and phosphorus thiochloride through esterification.Effects of solvents,the kinds of deacid reagent,the mol ratio of p-acetoamidophenol and phosphorus thiochloride,the dosage and composition of deacid reagent on the yield of TPTAA were studied.The results showed that the yield of TPTAA was 88.04% when the mole ratio of P-acetoamidophenol to triacetylamine+pyridine to trichlorothiophosDhate was 3.10:3.80:1,the mole ratio of triacetylamine to pyridine was 1:0.02,the temperature was 35℃ and the reaction time was 4 h.Then TPTA was synthesized by hydrolyzing TPTAA in acid condition,and the effect of the dosage of hydrochloric acid and methanol on the yield of tris(4-aminoDhenyl)thiophosphate(TPTA)was studied.The yield of TPTA was 95.62% when the mole ratio of methanol to hydrOChloric acid to TPTAA was 2.9:6.0:1,the temperature was 85℃ and the reaction time was 3 h.