HRID1797006

反应详情

EQUATION

反应方程式

HRID 1797006 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

trans-Cyclohexane-1,4-dicarboxylic acid dimethyl ester (34.2 g, 0.171 mol) was dissolved in 400 mL of anhydrous methanol and the solution brought to reflux. Slowly (dropwise), a solution of KOH (11.2 g, 0.171 mol, 85% purity) in dry methanol was added to the refluxing solution. The solution continued to reflux for 5 hours, and was then cooled and concentrated under reduced pressure to give a white solid. Water was added to dissolve most of the solid, and the aqueous mixture was washed with ether (3×) in a separatory funnel. The aqueous layer was brought to pH ˜6, the resulting white precipitate was collected via filtration and washed (1×) with a small amount of water. Air drying afforded trans-cyclohexane-1,4-dicarboxylic acid monomethyl ester as a white solid.

WORKUP

后处理

  1. temperatureto reflux
  2. temperatureto reflux for 5 hours
  3. temperaturewas then cooled
  4. concentrationconcentrated under reduced pressure
  5. customto give a white solid
  6. dissolutionto dissolve most of the solid
  7. washthe aqueous mixture was washed with ether (3×) in a separatory funnel
  8. filtrationthe resulting white precipitate was collected via filtration
  9. washwashed (1×) with a small amount of water
  10. customAir drying