HRID973423
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe reaction mixture was heated
- temperatureto reflux for 24 hours
- washThe reaction mixture was washed with 2×50 mL of NaOH
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated by rotary evaporation
- customThe residue was crystallized from isopropyl alcohol
- customto afford 5.5 g (75%) of analytically pure crystals, mp 158°-59° C.