HRID973423

反应详情

EQUATION

反应方程式

HRID 973423 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 50 mL of toluene was added 5.0 g (0.019 mol) of 4-(2-chloroethyl)-3,4-dihydro-2-methylpyrimido[1,6-a]benzimidazol-1(2H)-one, 6.19 g (0.038 mol) of 1-(2-pyridyl)piperazine, and 3.8 g (0.038 mol) of triethylamine. The reaction mixture was heated to reflux for 24 hours. The reaction mixture was washed with 2×50 mL of NaOH, dried over Na2SO4, filtered and concentrated by rotary evaporation. The residue was crystallized from isopropyl alcohol to afford 5.5 g (75%) of analytically pure crystals, mp 158°-59° C.

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 24 hours
  3. washThe reaction mixture was washed with 2×50 mL of NaOH
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated by rotary evaporation
  7. customThe residue was crystallized from isopropyl alcohol
  8. customto afford 5.5 g (75%) of analytically pure crystals, mp 158°-59° C.