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With N-chloro-succinimide In tetrachloromethane at 25 - 85℃; for 2 h;
Step 4: Synthesis of 5-chloro-1,3,4-thiadiazol-2-amine To a stirred solution of 1,3,4-thiadiazol-2-amine (0.5 g, 4.95 mmol) in CCl4 (10.0 mL), N-Chlorosuccinimide (0.73 g, 5.45 mmol) was added at 25° C. and reaction allowed to stir at 85° C. for 2 h. Reaction was monitored by TLC. On completion, reaction mixture was quenched with ice cold water and compound was extracted with 10percent methanol in DCM. The organic layer was washed with water, brine, dried over sodium sulphate and concentrated under reduced pressure to give crude. Purification of the compound was done by silica gel (100-200 mesh) column chromatography using 20percent ethyl acetate in hexane to give 5-chloro-1,3,4-thiadiazol-2-amine (0.18 g, 26.94percent) as light brown solid. MS: 135.97 [M++1].
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