HRID638728

反应详情

EQUATION

反应方程式

HRID 638728 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 4-nitrophenol (150 g, 1.079 moles), potassium carbonate (600 g, 4.341 moles) and sodium iodide (10 g, 66.7 mmol) in anhydrous acetone (2.1 L) was added methyl 6-bromohexanoate (156 g, 746.41 mmol) and heated to reflux for 48 hours. Acetone was distilled off and water (2 L) was added. Crude 39 was filtered, dried and recrystallised from a mixture of ethyl acetate:hexane (1:6) to get pure 39 (130 g, 45.1%) as a white powder. M.p: 84.5.5-86.6° C.

WORKUP

后处理

  1. temperatureheated
  2. temperatureto reflux for 48 hours
  3. distillationAcetone was distilled off
  4. additionwater (2 L) was added
  5. filtrationCrude 39 was filtered
  6. customdried
  7. customrecrystallised from a mixture of ethyl acetate:hexane (1:6)