HRID248062

反应详情

EQUATION

反应方程式

HRID 248062 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Suspend sodium hydride (10.1 g, 0.21 mol) in tetrahydrofuran (300 mL), place under a nitrogen atmosphere and cool to 0° C. Add, by dropwise addition, diethyl methylmalonate (34.8 g, 0.2 mol). Stir for 30 minutes at 0° C. and add 4-acetamidobenzyl chloride (38.6 g, 0.21 mol). Heat at reflux for 5 hours, cool and pour into water (400 mL). Extract with ethyl acetate (3×600 mL), dry (MgSO4) and evaporate the solvent in vacuo to give diethyl methyl-(4-acetamido)benzylmalonate.

WORKUP

后处理

  1. temperatureHeat
  2. temperatureat reflux for 5 hours
  3. temperaturecool
  4. extractionExtract with ethyl acetate (3×600 mL)
  5. dry with materialdry (MgSO4)
  6. customevaporate the solvent in vacuo