1-ethyl-1,3,5-triazine-2,4-dione → 1-Ethyl-1,3,5-triazinane-2,4-dione

Temperature

100 °C

To a quantity [370 gm., 2.62 mole] of the 1-ethyl-5-azauracil prepared in Part B, above is added 2200 ml. water and 40 gm. of 5 percent rhodium on activated charcoal. This mixture is put in a Parr hydrogenation chamber and hydrogen gas is introduced to a pressure of 50 pounds per square inch (p.s.i.) and the reaction system is heated to 100° C. When uptake of hydrogen ceases, the hydrogen pressure is increased to 200 p.s.i. and held there for 18 hours. The hydrogenated reaction mixture is rinsed out of the reaction chamber with hot water, filtered while hot, and the filter is washed with one liter of water at 80° C. The aqueous solution is set aside at 25° C. for 18 hours, during which interval crystals form. The crystals are collected on a filter and dried at 50° C. under reduced pressure. There is thus obtained 70 gm. of 5-ethyl-5,6-dihydro-s-triazine-2,4-(1H, 3H)-dione having a melting range between 220° C. and 224° C.

1. additionabove is added 2200 ml
2. additionis introduced to a pressure of 50 pounds per square inch (p.s.i.)
3. washThe hydrogenated reaction mixture is rinsed out of the reaction chamber with hot water
4. filtrationfiltered while hot, and the filter
5. washis washed with one liter of water at 80° C
6. waitThe aqueous solution is set aside at 25° C. for 18 hours, during which interval crystals form
7. customThe crystals are collected on
8. filtrationa filter
9. customdried at 50° C. under reduced pressure

ORD record

ord-5ed0b96df9a14e748371ccfe861ddc6a

Source dataset

uspto-grants-1983_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04423212