HRID632505

反应详情

EQUATION

反应方程式

HRID 632505 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 100 mL of ethanol were added 10.0 g of 1-methylpiperazine and 20.2 g of triethylamine. To the mixture cooled with ice, 25 mL of a solution of 24.6 g of 4-(bromomethyl)-2-methoxy-benzoic acid methyl ester in ethanol was added dropwise. The mixture was stirred at room temperature for 18 hours. The reaction mixture was concentrated. To the residue, 75 mL of water and 250 mL of methylene chloride were added, and the organic layer was separated. The obtained organic layer was dried over Na2SO4 and concentrated. The residue was purified by amino-silica gel column chromatography (heptane/AcOEt system) to give 22.4 g of the title compound (85% yield).

WORKUP

后处理

  1. additionwas added dropwise
  2. concentrationThe reaction mixture was concentrated
  3. additionTo the residue, 75 mL of water and 250 mL of methylene chloride were added
  4. customthe organic layer was separated
  5. dry with materialThe obtained organic layer was dried over Na2SO4
  6. concentrationconcentrated
  7. customThe residue was purified by amino-silica gel column chromatography (heptane/AcOEt system)