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ChemicalBook CAS DataBase List 2-AMINO-5-TERT-BUTYL-1,3,4-THIADIAZOLE

2-AMINO-5-TERT-BUTYL-1,3,4-THIADIAZOLE synthesis

6synthesis methods
-

Yield: 81%

Reaction Conditions:

with trichlorophosphate in toluene at 50 - 70; for 12 h;

Steps:

2; Formula 10 Synthesis of 2-amino-5-tert-butyl-1,3,4-thiadiazole (Compound P)
To install the thermometer, Stir the bar in a 2000 mL three-necked flask was added 109.4 g (1.20 mol) of thiosemicarbazide, 140 g (1.30 mol) of pivaloyl chloride, 800 mL toluene. 80 g (0.52 mol) of phosphorus oxychloride was added dropwise at 50 ° C, 70 deg C reaction 12 h, Cooled to room temperature, The reaction solution was poured into an ice-water mixture, A toluene solution containing 2-amino-5-tert-butyl-1,3,4-thiadiazole was separated, Distillation of concentrated toluene solution, The mixture was recrystallized from a mixed solvent of ethyl acetate and cyclohexane, To give 152.8 g of a white solid 2-amino-5-tert-butyl-1,3,4-thiadiazole, The purity of the liquid phase was 98.8% The yield was 81%.

References:

Xihua University;Liu, Ping;Yang, Weiqing;Ma, Menglin;Zhang, Yuanyuan;Zhang, Yan CN104530040, 2017, B Location in patent:Paragraph 0027; 0056; 0057

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