Synthesis of tris (4-aminophenyl) thiophosphate by amidehydrolysis method

Tris(4-acetamindophenyl) thiophosphate (TPTAA) was synthesized using p-acetoamidophe-nol and phosphorus thiochloride through esterification. Effects of solvents, the kinds of deacid rea-gent, 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 trichlorothiophosphate was 3. 10 : 3. 80 : 1, the mole ratio of triacetylamine to pyridine was 1 : 0. 02, the temperature was 35 °C 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-aminophenyl) 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 °C and the reaction time was 3 h.