HRID1907778

反应详情

EQUATION

反应方程式

HRID 1907778 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

Compound 549 (1.06 g, 3.68 mmol) and 1-methylpiperazine (0.818 mL, 7.37 mmol) were dissolved in toluene (40 mL) and stirred at 110° C. for 16 h. The toluene was removed on the rotary evaporator. The crude product was dissolved in ethyl acetate and washed with water. The organic layer was separated and dried with Na2SO4, filtered and concentrated via rotary evaporation. The residue was purified via Isco employing a 0 to 50% methanol:ethyl acetate solvent gradient to afford compound 550 (0.86 g, 66%) as a white solid.

WORKUP

后处理

  1. customThe toluene was removed on the rotary evaporator
  2. dissolutionThe crude product was dissolved in ethyl acetate
  3. washwashed with water
  4. customThe organic layer was separated
  5. dry with materialdried with Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated via rotary evaporation
  8. customThe residue was purified via Isco