Preparation method of phenylenediamine and phenylenediamine inorganic salt
A technology of phenylenediamine and inorganic salt, which is applied in the field of organic synthesis, can solve problems such as safe use, and achieve the effect of eliminating waste acid pollution and high yield
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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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