反应详情

During a 40 minute period, and at temperatures starting from 25° C. and ending at 47° C., 69.15 grams (0.580 mole) of methylaminoacetaldehyde dimethylacetate was added dropwise to a 300 ml benzene solution containing 143.3 g. (0.580 mole) of the 5-(1-phenoxyethyl)-1,3,4-thiadiazol-2-yl isocyanate isomer (prepared above) and the resulting solution was refluxed for 15 minutes to form a yellow solution. Hexane (1000 ml) was added and the resulting solution was heated on a steam bath, and then seeded with a few crystals of previously purified product. Upon cooling and standing overnight white crystals formed which were filtered, washed with hexane, air dried and then vacuum dried at 50° C. to give 171.4 grams of a powder of 3-[5-(1-phenoxyethyl)-1,3,4-thiadiazol-2-yl]-1-methyl-1-(2,2-dimethoxyethyl) urea. Melting point 117°-121° C.

1. customstarting from 25° C.
2. customending at 47° C.
3. additioncontaining 143.3 g
4. temperaturethe resulting solution was refluxed for 15 minutes
5. customto form a yellow solution
6. temperaturethe resulting solution was heated on a steam bath
7. temperatureUpon cooling
8. waitstanding overnight
9. customwhite crystals formed which
10. filtrationwere filtered
11. washwashed with hexane, air
12. customdried
13. customvacuum dried at 50° C.