HRID1973185

反应详情

EQUATION

反应方程式

HRID 1973185 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of methyl salicylate (6.4 ml., 7.6 g., 0.05 mole), 2,2,2-trifluoroethyl trifluoromethanesulfonate (13.9 g., 0.06 mole), anhydrous potassium carbonate (13.8 g., 0.1 mole) and acetone (150 ml.) is heated under reflux with efficient stirring for three days. The product is filtered and the filtrate is concentrated to a small volume. It is diluted with cold water and the resulting precipitate is collected and washed successively with cold dilute sodium hydroxide solution and water. The desired material is recrystallized then from aqueous ethanol to afford white solid, m.p. 61-62.

WORKUP

后处理

  1. temperatureis heated
  2. temperatureunder reflux
  3. filtrationThe product is filtered
  4. concentrationthe filtrate is concentrated to a small volume
  5. additionIt is diluted with cold water
  6. customthe resulting precipitate is collected
  7. washwashed successively with cold dilute sodium hydroxide solution and water
  8. customThe desired material is recrystallized
  9. customfrom aqueous ethanol to afford white solid, m.p. 61-62