HRID2097359

反应详情

EQUATION

反应方程式

HRID 2097359 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
95 °C

PROCEDURE

实验过程

4-(2-Morpholin-4-yl-ethoxy)-phenol (3.39 g, 15.2 mmol), N-(6-bromohexyl)-phthalimide (4.72 g, 15.2 mmol) and K2CO3 (4.20 g, 30.4 mmol) were suspended in DMF (35 mL) under an atmosphere of argon and stirred at 95° C. for 17 h. The solvent was evaporated under reduced pressure and the residue was partitioned between water (150 mL) and CH2Cl2 (150 mL). The aqueous layer was extracted with CH2Cl2 (2×100 mL), the combined org. layers were dried over Na2SO4, filtered and the solvent was removed under reduced pressure. The residue was purified by flash chromatography (EtOAc) to give the title compound together with some starting phenol (≈2:1). The mixture was used for subsequent reactions without further purification.

WORKUP

后处理

  1. customThe solvent was evaporated under reduced pressure
  2. customthe residue was partitioned between water (150 mL) and CH2Cl2 (150 mL)
  3. extractionThe aqueous layer was extracted with CH2Cl2 (2×100 mL)
  4. dry with materiallayers were dried over Na2SO4
  5. filtrationfiltered
  6. customthe solvent was removed under reduced pressure
  7. customThe residue was purified by flash chromatography (EtOAc)