反应详情

A 200 milliliter flask was charged with 2.1 grams (0.018 mole) of methylaminoacetaldehyde dimethylacetal, 50 milliliters of benzene and 5.8 grams (0.018 mole) of the 5-[1-(2,4-dichlorophenoxy)ethyl]-1,3,4-thiadiazol-2-yl isocyanate dimer (prepared above). The resulting slurry was refluxed for 15 minutes to form a yellow solution and cooled with formation of a few crystals. A minimum amount of hexane-diethylether was added, and crystallization occurred. The crystals were filtered off, and dried in a vacuum oven at 80°0 C. to give 6.4 grams of white crystals of 3-[5-[1-(2,4-dichlorophenoxy)-ethyl]-1,3,4-thiadiazol-2-yl]-1-methyl-1-(2,2-dimethoxyethyl)urea. (Melting point 125°-127° C.).

1. temperatureThe resulting slurry was refluxed for 15 minutes
2. customto form a yellow solution
3. temperaturecooled with formation of a few crystals
4. customcrystallization
5. filtrationThe crystals were filtered off
6. customdried in a vacuum oven at 80°0 C