A kind of preparation method of phenylenediamine and phenylenediamine inorganic salt
A technology of phenylenediamine and inorganic salt, applied in the field of organic synthesis, can solve problems such as safe use
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Embodiment 1
[0041] The synthesis of iso-terephthaloyl hydroxamic acid: with reference to the literature synthesis method (Li Aixiu et al., Applied Chemistry, 2004, Volume 21, Phase 1, pages 87-89), with dimethyl isophthalate, Dimethyl terephthalate, hydroxylamine hydrochloride and potassium hydroxide were used as raw materials to obtain isophthaloyl hydroxamic acid and terephthaloyl hydroxamic acid (yield>95%), respectively. Infrared characteristic peaks: 3294, 2751, 1654, 1616, 1558cm -1 , consistent with the data and maps reported in the literature.
Embodiment 2
[0043] Synthesis of potassium salt of isophthaloyl hydroxamic acid:
[0044] At 20-25°C, add 28g of potassium hydroxide aqueous solution (28g / 35mL) into hydroxylamine hydrochloride solution (17.4g of hydroxylamine hydrochloride / 30mL of methanol and 30mL of water), and mix well to obtain a hydroxylamine solution, then at 20-25°C, add The hydroxylamine solution was slowly added dropwise to a methanol solution of dimethyl isophthalate (19.42 g / 160 mL methanol). After stirring for 2.5-3.0 hours, all solvents were directly evaporated to dryness without adding acid to neutralize the reaction solution. Then wash the solid product with 80mL of methanol-acetone (1:1v / v), dry to obtain the potassium salt of isophthaloyl hydroxamic acid, 35.6g of light yellow solid (containing KCl), infrared characteristic peaks: 3264, 1655, 1625cm -1 .
[0045] Synthesis of Potassium Terephthaloyl Hydroxamic Acid:
[0046] In the same way, the above dimethyl isophthalate is replaced by dimethyl terep...
Embodiment 3
[0048] The synthesis of p-phenylenediamine: in 50mL pressure reactor, put into the potassium salt of terephthaloyl hydroxamic acid (0.2g) and acetonitrile-water mixture (2mL, 1.5:1v / v ), heat up to 155°C (oil bath temperature) after pumping and sealing the test tube. After 1 hour of reaction, the yellow suspension turned into a purple solution. After cooling down, the reaction solution was neutralized with dilute hydrochloric acid, and then extracted with ethyl acetate. Solvent was evaporated to dryness to obtain p-phenylenediamine (90% of productive rate, and productive rate is calculated based on phthaloyl hydroxamic acid potassium salt, productive rate=actual yield / theoretical yield), thin-layer chromatographic analysis is a single product, no raw material Residue, its infrared spectrum is consistent with the standard sample.
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