5-(2-FLUORO-BENZYL)-[1,3,4]THIADIAZOL-2-YLAMINE synthesis

Yield:39181-53-8 89%

Reaction Conditions:

Stage #1: thiosemicarbazide;(2-fluorophenyl)acetic acidwith trichlorophosphate at 75; for 2 h;
Stage #2: in water at 110; for 4 h;

Steps:

1 Example 1: Synthesis of intermediate 5-(2-fluorobenzyl)-1,3,4-thiadiazol-2-amine (3).

Add 15mmol 2-fluorophenylacetic acid and 15mmol thiosemicarbazide into a 100ml round bottom flask, put the round bottom flask into an oil bath, and use a 3ml disposable plastic-tip dropper to suck up 7.5ml of phosphorus oxychloride after adding it Reflux at 75°C for 2 hours, take out the round-bottomed flask and let it stand, cool to room temperature, add 45ml of water, reflux at 110°C for 4 hours, take it out and let it stand, adjust the pH to above 8 with 60% sodium hydroxide, and pump while hot After filtration, the filter cake was washed with water to neutrality, dried and recrystallized with methanol, filtered and dried to obtain a white solid with a yield of 89%.

References:

CN113527225,2021,A Location in patent:Paragraph 0024-0026