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

Yield:39181-52-7 74%

Reaction Conditions:

with trichlorophosphate at 75; for 6 h;Cooling with ice;

Steps:

Synthesis of 5-(substituted-phenethyl)-1,3,4- thiadiazol-2-amines;general procedure

General procedure: POCl3 (0.28 mol) was added dropwise to a mixture of the substituted phenylacetic acid (0.07 mol) with thiosemicarbazide (0.105 mol) in an ice bath. Then the reaction mixture was refluxed over an oil bath for 6 h. The reaction was monitored by TLC. When the reaction was completed and cooled to room temperature, water (100 mL) was added to the reaction mixture and refluxed for 1h. After cooling, the mixture was basified to pH 8-9 by the dropwise addition of 50%NaOH solution under an ice bath. The precipitate was filtered and recrystallised from ethanol to obtain the compounds.

References:

Zhu, Hui-Long;Liu, Yu-Wei;Liu, Wei-Wei;Yin, Fu-Jun;Cao, Zhi-Ling;Bao, Juan;Li, Meng;Qin, Ling-Yan;Shi, Da-Hua [Journal of Chemical Research,2016,vol. 40,# 1,p. 16 - 20]