HRID1292133

反应详情

EQUATION

反应方程式

HRID 1292133 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To 3-hydroxybenzamide (274 mg; 2.0 mM) under a nitrogen atmosphere was added potassium carbonate (276 mg; 21.0 mM). This was dissolved in acetonitrile (20 ml) containing allyl bromide (169 ul; 2.0 mM). The mixture was refluxed for 5 hours, and the reaction followed by T.L.C.: 10% MeOH: 90% CH2Cl2. The excess solvent was then removed under vacuum, the organics extracted into dichloromethane, dried, and the solvent removed, to yield a white solid. This was recrystallised from hot water to produce a white "needle" solid (63%) as the final product.

WORKUP

后处理

  1. temperatureThe mixture was refluxed for 5 hours
  2. customThe excess solvent was then removed under vacuum
  3. extractionthe organics extracted into dichloromethane
  4. customdried
  5. customthe solvent removed
  6. customto yield a white solid
  7. customThis was recrystallised from hot water