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In a mixture of 9.66 g of sodium hydroxide, 14.6 ml of water, and 122 of methanol was dissolved 36.3 g of 2,5-dimercapto-1,3,4-thiadiazole. After cooling the mixture, a solution of 24.1 ml of ethyl bromoacetate and 24 ml of methanol was added to the mixture below 10° C. The resultant mixture was stirred for 3 hours at room temperature and cooled below 10° C. 43.5 ml of water and 400 ml of 50% methanol were successively added to the reaction mixture, whereby crystals precipitated, and the mixture was allowed to stand overnight at 4° C. The crystals were collected by filtration, washed successively with water and then 50% methanol, and dried to provide 42.5 g of ethyl [(5-mercapto-1,3,4-thiadiazol-2-yl)thio]acetate.

1. temperatureAfter cooling the mixture
2. temperaturecooled below 10° C
3. customprecipitated
4. filtrationThe crystals were collected by filtration
5. washwashed successively with water
6. dry with material50% methanol, and dried