HRID1279203

反应详情

EQUATION

反应方程式

HRID 1279203 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 2,4-dihydro-4-[4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl]-3H-1,2,4-triazol-3-one (0.05 mol) prepared as described in Eβ-A-0,006,711, 3-bromo-2-pentanone (0.073 mol) and K2CO3 (10 g) in DMF (200 ml) and toluene (200 ml) was stirred and refluxed overnight using a water separator. The solvent was evaporated. The residue was dissolved in CH2Cl2. The organic solution was washed, dried, filtered and the solvent was evaporated. The residue was crystallized from 2-propanol. The precipitate was filtered off and the filtrate was evaporated. The residue was triturated in DIPE, filtered off and dried, yielding 4.6 g of (±)-2-(1-ethyl-2-oxopropyl)-2,4-dihydro-4-[4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl]-3H-1,2,4-triazol-3-one (intermn.

WORKUP

后处理

  1. customprepared
  2. temperaturerefluxed overnight
  3. customThe solvent was evaporated
  4. dissolutionThe residue was dissolved in CH2Cl2
  5. washThe organic solution was washed
  6. customdried
  7. filtrationfiltered
  8. customthe solvent was evaporated
  9. customThe residue was crystallized from 2-propanol
  10. filtrationThe precipitate was filtered off
  11. customthe filtrate was evaporated
  12. customThe residue was triturated in DIPE
  13. filtrationfiltered off
  14. customdried