Preparation method of isoluminol CAS NO.3682-14-2

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Chemiluminescence refers to the phenomenon of emitting visible light in some special chemical reactions. Its luminescence mechanism is that the chemical substances in the reaction system absorb the energy released by the reaction and transition from the ground state to the excited state, so as to produce chemiluminescence. Isoluminol（   4-phthaloyl hydrazide) reagents have high luminescence quantum yield and good water solubility, and can react with a variety of oxidants to produce chemical light, so they are widely used in the fields of food, environment, criminal investigation, medicine and so on.

The method for preparing isoluminol from Phthalic hydrazide (which must be carried out at room temperature) comprises the following steps:

Step 1: preparation of diacetyl Phthaloyl hydrazide

First prepare a 500ml flask, add 60g of dry (40%) Phthaloyl hydrazide waste and 200ml of acetic acid to the flask, stir evenly, then add 30g of sodium acetate, stir again for 30 minutes, slowly drop 40g of acetyl chloride within 30 minutes, stir for 1 hour, put it into a heating box, adjust it to 70 ℃ for reaction for 5 hours, take out the solution and naturally reduce it to room temperature.

Step 2: prepare nitroso diacetyl Phthaloyl hydrazide

Add 15g sodium nitrite into the solution in step 1 in batches, mix and stir for 3 hours, distill under reduced pressure to recover acetic acid to obtain the crude 4-nitrosodiaacetyl Phthaloyl hydrazide,

Step 3: prepare nitroso Phthaloyl hydrazide

Add 200ml 95v / v% ethanol to the crude 4-nitrosodiaacetyl Phthaloyl hydrazide, mix well, and add 10g sodium hydroxide in batches. After addition, the reaction was heated and refluxed for 5 hours to obtain the required solution.

Step 4: prepare isoluminol

Add 10g sodium thiosulfate to the solution obtained in the previous step at one time and stir for 30 minutes. After heating and refluxing for 3 hours, the reaction solution is naturally reduced to room temperature, then filtered and the filter cake is collected. 95% ethanol is recovered by rotary distillation of the filtrate, the residue is combined with the filter cake, added to 200ml water, heated to 80 ℃, stirred for 30 minutes, and filtered while hot. Add concentrated hydrochloric acid to the filtrate, adjust the pH to 9, and cool naturally for crystallization. After filtration, 26G light yellow powdered isoluminol product was obtained.