HRID896480

反应详情

EQUATION

反应方程式

HRID 896480 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Dissolve 4-hydroxybenzaldehyde (0.082 mol) in dimethylformamide (100 ml) and add potassium carbonate (0.164 mol) and 1-bromo-2-chloroethane (0.246 mol). Stir magnetically for five days at ambient temperature, then hydrolyse the reaction mixture in 500 ml of water and render alkaline with 3 g of sodium hydroxide pellets. Extract twice with 50 ml of ether each time. Dry the organic phase over magnesium sulphate and remove the ether by evaporation under reduced pressure. Purify the resulting oil by flash chromatography using a 9/1 cyclohexane/ether mixture as eluant. Subsequently, remove the mixture of solvents by evaporation under reduced pressure and crystallise the resulting yellow oil and store it in a dessicator.

WORKUP

后处理

  1. extractionExtract twice with 50 ml of ether each time
  2. dry with materialDry the organic phase over magnesium sulphate
  3. customremove the ether
  4. customby evaporation under reduced pressure
  5. customPurify the resulting oil by flash chromatography
  6. customSubsequently, remove
  7. additionthe mixture of solvents
  8. customby evaporation under reduced pressure
  9. customcrystallise the resulting yellow oil and store it in a dessicator