酰胺水解法合成硫代磷酸三(4-氨基苯)酯

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4h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3h时,TPTA的收率95.62%。

SYNTHESIS OF TRIS(4-AMINOPHENYL)THIOPHOSPHATE BY AMIDEHYDROLYSIS METHOD

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.