반응 #63700

반응 방정식

water

1-[2,4-dichloro-5-(1-methylethoxy)phenyl]-3,3-dimethyl-1,2,4-triazolidin-5-one

pyruvic acid

pyruvic acid

→

2-[2,4-dichloro-5-(1-methylethoxy)phenyl]-6-methyl-1,2,4-triazine-3,5(2H,4H)-dione

수율 58.6%

용매

p-dioxane

반응 조건

후처리

1. 1
   온도The mixture was heated at 90° C. for three hours
2. 2
   추출The mixture was extracted with ethyl acetate
3. 3
   기타the solvent was evaporated from the
4. 4
   추출extract under reduced pressure
5. 5
   기타to give an oil
6. 6
   기타The oil was purified by thin-layer preparative chromatography on silica gel
7. 7
   세척eluting with ethyl acetate:heptane (1:1)
8. 8
   추출Extraction of the appropriate bands

실험 절차

To a stirred mixture of 1.0 g (0.0031 mole) of 1-[2,4-dichloro-5-(1-methylethoxy)phenyl]-3,3-dimethyl-1,2,4-triazolidin-5-one in 10 mL of p-dioxane was added 0.29 g (0.0031 mole) of pyruvic acid and one drop of concentrated sulfuric acid. The mixture was stirred at room temperature for one hour, then an additional 0.25 g (0.0029 mole) of pyruvic acid was added. The mixture was heated at 90° C. for three hours, then poured into water. The mixture was extracted with ethyl acetate, and the solvent was evaporated from the extract under reduced pressure to give an oil. The oil was purified by thin-layer preparative chromatography on silica gel, eluting with ethyl acetate:heptane (1:1). Extraction of the appropriate bands gave 0.6 g of 2-[2,4-dichloro-5-(1-methylethoxy)phenyl]-6-methyl-1,2,4-triazine-3,5(2H,4H)-dione as a solid (mp 163°-164° C.), Compound 10 in the tables.

출처