5-(2-IODO-PHENYL)-[1,3,4]THIADIAZOL-2-YLAMINE synthesis

Yield:299934-10-4 98.9%

Reaction Conditions:

with choline chloride;urea at 80; for 2 h;

Steps:

5.1-5.3 Example 5Preparation of 2-amino-5- (2-iodophenyl) -1,3,4-thiadiazole

In the first step, 1 mol of choline chloride and 2 mol of urea are added to the reaction vessel.Stir at 80 ° C until fully dissolved to obtain a eutectic solvent;In the second step, after the reaction system is cooled to room temperature, 1 mol of o-iodobenzoic acid and 1.2 mol of thiosemicarbazide are added, the temperature is slowly raised, and the reaction is refluxed at 80 ° C for 2 hours.TLC monitors the end of the reaction;In the third step, the reaction mixture is cooled to room temperature, and then the pH value is adjusted to 8-9 with a 10% aqueous ammonia solution under ice-cooling, a solid is precipitated, filtered with suction, and the filter cake is washed with ice waterDrying to give 2-amino-5- (2-iodophenyl) -1,3,4-thiadiazole in a yield of 98.9%. The filtrate was recovered to obtain a eutectic solvent.

References:

CN110724115,2020,A Location in patent:Paragraph 0066-0072