反应详情

At ambient temperatures 3.9 grams (0.033 mole) of methylaminoacetaldehyde dimethylacetate was slowly added to a 30 ml. benzene solution containing 9.2 grams (0.033 mole) of the 5-[1-(4-chlorophenoxy)ethyl]-1,3,4-thiadiazol-2-yl isocyanate dimer (prepared above). The resulting solution was refluxed for 30 minutes to form a yellow solution and then cooled and topped with a roto-vac at 60 degrees centigrade to 12.4 grams of a viscous yellow oil which crystallized upon standing. The entire sample was recrystallized from a minimum amount of ethylacetate/hexane solution. The crystals were filtered off, and dried in a vacuum oven at 80 degrees centigrade to give 8.3 grams of fluffy white crystals of 3-[5-[1-(4-chlorophenoxy)ethyl-]-1,3,4-thiadiazol-2-yl]-1-methyl-1-1(2,2-dimethoxyethyl)urea. Melting point 116-118 degrees centigrade.

1. temperatureThe resulting solution was refluxed for 30 minutes
2. customto form a yellow solution
3. temperaturecooled
4. customcrystallized
5. customThe entire sample was recrystallized from a minimum amount of ethylacetate/hexane solution
6. filtrationThe crystals were filtered off
7. customdried in a vacuum oven at 80 degrees centigrade