2-Amino-5-methyl-1,3,4-thiadiazole synthesis
- Product Name:2-Amino-5-methyl-1,3,4-thiadiazole
- CAS Number:108-33-8
- Molecular formula:C3H5N3S
- Molecular Weight:115.16
Yield:108-33-8 96.3%
Reaction Conditions:
with choline chloride;urea at 80; for 1 h;
Steps:
1.1-1.3 Example 1Preparation of 2-amino-5-methyl-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 cooling the reaction system to room temperature, 1 mol of acetic acid and 1.2 mol were added.Thiosemicarbazone, slowly heating, refluxing at 80 ° C for 1h,TLC monitors the end of the reaction;The third step is to cool the reaction mixture to room temperature.Then adjust the pH to 8-9 with 10% ammonia solution under ice-bath cooling.The solid precipitated out, filtered with suction, the filter cake was washed with ice water, and then recrystallized.Obtained 2-amino-5-methyl-1,3,4-thiadiazole, yield 96.3% the filtrate was recovered to obtain a eutectic solvent.
References:
CN110724115,2020,A Location in patent:Paragraph 0038-0044
