反应详情

温度

-75 °C

A mixture of 2,6-dichloro-α-(4-chlorophenyl)-4-(4,5-dihydro-3,5-dioxo-1,2,4,-triazin-2(3H)-yl)-benzeneacetyl chloride (0.05 mol) in THF (200 ml) was stirred at −75° C. A solution of chloroethyl magnesium (0.1 mol; 2 M/THF) in THF (50 ml) was added dropwise at −75° C. The reaction mixture was stirred for 90 minutes, then the temperature was raised to −20° C. A saturated aqueous NH4Cl solution was added dropwise. Water was added and the product was extracted with CH2Cl2. The organic layer was separated, dried, filtered and the solvent was evaporated. The residue was filtered over silica gel (eluent: CH2Cl2/CH3OH 98/2). Two fractions were collected and the solvent was evaporated, yielding 3.8 g (±)-2-[3,5-dichloro-4-[1-(4-chlorophenyl)-2-oxobutyl]phenyl]-1,2,4-triazine-3,5(2H,4H)-dione (interm. 69).

1. stirringThe reaction mixture was stirred for 90 minutes
2. temperaturethe temperature was raised to −20° C
3. extractionthe product was extracted with CH2Cl2
4. customThe organic layer was separated
5. customdried
6. filtrationfiltered
7. customthe solvent was evaporated
8. filtrationThe residue was filtered over silica gel (eluent: CH2Cl2/CH3OH 98/2)
9. customTwo fractions were collected
10. customthe solvent was evaporated