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ChemicalBook CAS DataBase List 2-AMINO-5-BROMO-[1,3,4]THIADIAZOLE

2-AMINO-5-BROMO-[1,3,4]THIADIAZOLE synthesis

2synthesis methods
-

Yield:37566-39-5 85%

Reaction Conditions:

Stage #1:formic acid;thiosemicarbazide with sulfuric acid in water for 3 h;Reflux;
Stage #2: with ammonium hydroxide;bromine in water; pH=3.5 - 8
Stage #3: in water

Steps:


5-bromo-l, 3, 4-thiadiazol-2-amine VI1 mol of V was suspended in 50 ml of 85% water formic acid and 80 ml of sulfuric acid were carefully added. Reaction mixture was stirred for 3 hours on boiling water bath and then cooled down. 800 ml of water were added and reaction mixture was alkalified by water ammonia solution to ph 3.5. Then reaction mixture was heated to 550C and 68.5 ml of Br2 were added dropwise under liquid layer, keeping on temperature 550C and ph 3.5. Reaction mixture was stirred at this temperature overnight and after that it was cooled down and basified by water ammonia solution to ph 8. Precipitate which was formed was filtered off, washed by water and dried to provide title compound 153.02 g (85%).

References:

URIFER LTD.;NIR, Uri;SHPUNGIN, Sally;YAFFE, Etai;COHEN, Moshe WO2010/97798, 2010, A1 Location in patent:Page/Page column 17

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