Isotope element 15N labeled melamine and method for synthesizing derivatives thereof
A melamine and synthesis method technology, applied in the direction of organic chemistry, etc., can solve the problems of difficult product separation, complex process, low utilization rate of raw materials, etc., and achieve the effects of high utilization rate, simple method process, good economy and use value
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Embodiment 1
[0042] isotope 15 The synthetic method of N mark melamine (structural formula three):
[0043] Add 7.38g of cyanuric acid and 72ml of dioxane into the stainless steel reaction kettle and seal it. After being put into an ice-water bath and stirring for 10 minutes, add 40ml of dilute ammonia water (containing 17.31g of concentration 25% 15 N-ammonia) solution, sealed. Put it in an oil bath and heat it to 130°C, and react for 4h. After the reaction was completed, the reaction solution was evaporated to dryness, recrystallized, filtered, and dried to obtain 5.10 g of white solid: 15 N 3 - Melamine (in the substituent 15 N mark, as shown in structural formula three), reclaim NH 4 After Cl, with 15 The yield of N raw material is 98%. HPLC detection, purity ≥ 99%; mass spectrometry detection, abundance ≥ 98% atom 15 N.
Embodiment 2
[0045] isotope 15 The synthetic method of N mark melamine (structural formula four):
[0046] 7.50g 15 N 3-Add cyanuric acid and 72ml of dioxane into the stainless steel reaction kettle, and seal it. Put it in an ice-water bath and stir for 10 minutes, add 40 ml of dilute ammonia water (containing 18.g of 25% ammonia water) solution from the feed valve of the reaction kettle, and seal it. Put it in an oil bath and heat it to 130°C, and react for 4h. After the reaction was completed, the reaction solution was evaporated to dryness, recrystallized, filtered, and dried to obtain 5.19 g of white solid: 15 N 3 - Melamine (in the triazine ring 15 N marks, such as structural formula 4), with 15 The yield of N raw material is 99.8%. HPLC detection, purity ≥ 99%; mass spectrometry detection, abundance ≥ 98% atom 15 N.
Embodiment 3
[0048] isotope 15 N labeled melamine derivatives——2- 15 The synthetic method of N-amino-4,6-dichloro-1,3,5-triazine:
[0049] Add 3.69g of cyanuric acid and 36ml of acetone into a 250ml two-necked flask with a condenser, put it in an ice-water bath with vigorous stirring, and add 5ml of 2.88g of 25% concentration dropwise. 15 N-ammonia. After the dropwise addition, the reaction temperature was maintained at 0°C for 4h. After the reaction was completed, the product was filtered with suction, washed with deionized water, and dried to obtain 2.99g of white solid: 2- 15 N-Amino-4,6-dichloro-1,3,5-triazine, recovered NH 4 After Cl, with 15 Based on N raw materials, the yield is 90%. HPLC detection, purity ≥ 99%; mass spectrometry detection, abundance ≥ 98% atom 15 N.
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