反应详情

温度

175 °C

A mixture of 4.2 parts of 2-[4-[(4-chlorophenyl)cyanomethyl]-3-methoxyphenyl]-2,3,4,5-tetrahydro-3,5-dioxo-1,2,4-triazine-6-carboxylic acid and 13 parts of 2-mercaptoacetic acid is stirred and heated for 2 hours at 175° C. After cooling, 150 parts of water are added. The aqueous phase is decanted and the remaining oil is stirred in water. The whole is treated with sodium hydrogen carbonate. The product is extracted with a mixture of trichloromethane and methanol (90:10 by volume). The extract is dried, filtered and evaporated. The residue is purified by column chromatography over silica gel using a mixture of trichloromethane and methanol (97:3 by volume) as eluent. The pure fractions are collected and the eluent is evaporated in vacuo. The residue is crystallized from 8 parts of acetonitrile. The product is filtered off, washed with 2,2'-oxybispropane and dried, yielding α-(4-chlorophenyl)-4-(4,5-dihydro-3,5-dioxo-1,2,4-triazin-2(3H)-yl)-3-methoxybenzeneacetonitrile (intermediate 2).

1. temperatureAfter cooling
2. customThe aqueous phase is decanted
3. stirringthe remaining oil is stirred in water
4. additionThe whole is treated with sodium hydrogen carbonate
5. extractionThe product is extracted with a mixture of trichloromethane and methanol (90:10 by volume)
6. customThe extract is dried
7. filtrationfiltered
8. customevaporated
9. customThe residue is purified by column chromatography over silica gel using
10. additiona mixture of trichloromethane and methanol (97:3 by volume) as eluent
11. customThe pure fractions are collected
12. customthe eluent is evaporated in vacuo
13. customThe residue is crystallized from 8 parts of acetonitrile
14. filtrationThe product is filtered off
15. washwashed with 2,2'-oxybispropane
16. customdried